CN108493305B - A kind of preparation method of graphical sapphire substrate - Google Patents

A kind of preparation method of graphical sapphire substrate Download PDF

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Publication number
CN108493305B
CN108493305B CN201810242244.9A CN201810242244A CN108493305B CN 108493305 B CN108493305 B CN 108493305B CN 201810242244 A CN201810242244 A CN 201810242244A CN 108493305 B CN108493305 B CN 108493305B
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sapphire substrate
etch resistant
resistant coating
preparation
graphical sapphire
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CN108493305A (en
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孙逊运
周元基
于凯
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WEIFANG XINGTAIKE MICROELECTRONIC MATERIALS CO Ltd
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WEIFANG XINGTAIKE MICROELECTRONIC MATERIALS CO Ltd
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/005Processes

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  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
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Abstract

The present invention relates to semiconductors manufactures, more particularly, to a kind of preparation method of graphical sapphire substrate.The preparation method includes the following steps: that (a) coats to form etch resistant coating in sapphire substrate surface;(b) siliceous photoresist is coated in etch resistant coating surface and form siliceous photoresist layer, be lithographically formed mask pattern;(c) etch resistant coating is etched under the protection of siliceous photoresist layer, and mask pattern is transferred to etch resistant coating;(d) siliceous photoresist is removed;(e) etch resistant coating and Sapphire Substrate are etched, the graphical sapphire substrate is obtained.The present invention uses the siliceous photoresist combination etch resistant coating of ultrathin, not only has high etch resistance energy, but also equally ensure that high resolution ratio and yield requirement by contact exposure, is effectively controlled equipment cost.

Description

A kind of preparation method of graphical sapphire substrate
Technical field
The present invention relates to semiconductors manufactures, more particularly, to a kind of preparation method of graphical sapphire substrate.
Background technique
Mechanical performance and chemical stability are good, do not absorb visible light, manufacturing technology relative maturity because having for Sapphire Substrate The advantages that, it is the ideal substrate material of LED.Graphical sapphire substrate (Patterned Sapphire Substrate, Abbreviation PSS), it is to produce the micro structured pattern with ad hoc rules in process for sapphire-based plate surface in a manner of corroding or etch, To effectively increase the optical output power and luminous efficiency of LED.
The PSS substrate figure of mainstream is bottom edge diameter about 2um at present, is spaced about 1um, and height is about the circle of 1.5-1.8um Cone.For the resolution ratio and process yields for guaranteeing micrometer structure figure, complicated stepping projection is generallyd use in PSS manufacturing process Formula exposure method needs default exposure area, camera lens focal plane and projection ratio, carries out subregion projection exposure.The technique is to photoetching The performance requirements such as the etch resistance of glue are very high, and most of photoresists do not reach requirement, and cannot be considered in terms of resolution ratio and etch resistance energy.
In the prior art, have and gradually deposit silicon dioxide film and ITO etc. on a sapphire substrate, pass through high annealing or change Reaction is learned, particle is formed on surface, PSS substrate is then formed by etching, but this method is difficult to ensure in production process Distributing homogeneity, and being repeated cyclically property is poor, cannot achieve industrialized production substantially.Also there is the method pair using multiple etching PSS substrate performance and etching technics are improved, but at least to carry out 3 times or more etching process, considerably increase work Skill complexity and production cost.
In addition, in the prior art, also there is the figure for attempting nano-imprint method and holographic exposure method to realize Sapphire Substrate Change, nano impression is contact, has extremely harsh requirement to nano-form and substrate parallelism, demoulding, exhaust and mother matrix Pollution can make the yield of volume production very uncontrollable;And holographic exposure method, Gaussian hot spot uniformity and environment oscillation Figure quality is seriously affected, it is made to be difficult to ensure the yield of product and lot stability.
In view of this, the present invention is specifically proposed.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of graphical sapphire substrate, to solve to exist in the prior art The problem of complex process when preparing graphical sapphire substrate, high production cost.
In order to realize above-mentioned purpose of the invention, the following technical scheme is adopted:
A kind of preparation method of graphical sapphire substrate, includes the following steps:
(a) it coats to form etch resistant coating in sapphire substrate surface;
(b) siliceous photoresist is coated in etch resistant coating surface and form siliceous photoresist layer, be lithographically formed mask pattern;
(c) etch resistant coating is etched under the protection of siliceous photoresist layer, and mask pattern is transferred to etch resistant coating;
(d) siliceous photoresist is removed;
(e) etch resistant coating and Sapphire Substrate are etched, the graphical sapphire substrate is obtained.
Preferably, the silicone content of the siliceous photoresist is 30%-45%.It is furthermore preferred that the silicon of the siliceous photoresist Content is 40%-42%.
Siliceous photoresist has good etch resistance energy, and is clearly distinguishable from the etching ratio of organic etch resistant coating, Therefore thickness control can meet the requirement of etch resistance energy in 100 nanometer level, and ultra-thin film thickness can be exposed using contact Light mode forms mask pattern, and avoiding common thick film photoresist, in contact exposure, existing resolution ratio is low, has standing wave effect It answers, the problem that poor contrast, figure consistency difference etc. cause yield low.
Preferably, the photoresist layer with a thickness of 50-500nm.It is furthermore preferred that the photoresist layer with a thickness of 80- 150nm。
Preferably, the etch resistant coating is organic etch resistant material.Conventional organic etch resistant material, etch resistant can be selected Coating is without having photosensitive property, and light source is served as a contrast through after photoresist thin layer in sapphire when can reduce exposure using one side Reflex on bottom;On the other hand, avoid siliceous photoresist layer and Sapphire Substrate directly contacts that there are etching selections Than the problem of difference, etching efficiency is improved.It is furthermore preferred that organic etch resistant material includes thermosetting resin.It is further excellent Choosing, organic etch resistant material further includes curing agent.
Corresponding curing agent is added in thermosetting resin, can be improved the curing rate of etch resistant material, guarantees solidification The compactness of product structure improves the etch resistance energy of etch resistant coating.
Preferably, the etch resistant coating with a thickness of 1-3 μm.It is furthermore preferred that the etch resistant coating with a thickness of 1.5-2.5μm。
Preferably, in the step (b), mask pattern is formed on photoresist layer by yellow light technique, specifically, described Siliceous photoresist is toasted by yellow light technique, is exposed, being developed, and forms required litho pattern.Preferably, it exposes Mode can be needed to carry out subregion multistep and be swept using primary complete molding contact exposure when avoiding existing projection exposure It retouches exposure, complex process and time-consuming and there is have the problem of stitching error easily causes pattern deformation between visual field.
Preferably, mask pattern is transferred to by etch resistant by plasma etching etch resistant coating in the step (c) Coating.It is furthermore preferred that containing oxygen element in the plasma etching gas.Since etch resistant coating main component is hydrocarbon Oxygen organic compound, and photoetching offset plate figure layer main component is silicon and oxygen, therefore uses conventional oxygen-containing etching gas can be light The easy etch resistant coating etched away not under the protection of photoetching offset plate figure layer.
Preferably, siliceous photoresist layer is removed by plasma etching in the step (d).It is furthermore preferred that described etc. Plasma etching gas contains fluorine element.The silicon content of siliceous photoresist layer is about 40%, and ingredient is adopted already close to silica Photoresist layer can be etched away with conventional fluorine-containing etching gas atmosphere.
Preferably, pass through sense coupling etch resistant coating and Sapphire Substrate in the step (e).More Preferably, the etching gas is Cl2And BCl3.Sense coupling is high-efficient, and etching injury is small, and uniformity is good, It is at low cost.By above-mentioned condition, the etch rate that ICP mode etches Sapphire Substrate can be improved.
Compared with prior art, the invention has the benefit that
(1) preparation method of graphical sapphire substrate of the invention, using siliceous photoresist combination etch resistant coating It uses, increases etch resistance energy, and thin photoresist thickness makes contact exposure mode equally and can satisfy technique to resolution The high request of rate and yield;
(2) preparation method simple process of the invention, the period is reproducible, and production cost is low;
(3) preparation method of the invention, can according to actual needs, and transfer mask figure obtains different targeted graphicals Sapphire Substrate pattern, it is adaptable.
Detailed description of the invention
It, below will be to specific in order to illustrate more clearly of the specific embodiment of the invention or technical solution in the prior art Embodiment or attached drawing needed to be used in the description of the prior art be briefly described, it should be apparent that, it is described below Attached drawing is some embodiments of the present invention, for those of ordinary skill in the art, before not making the creative labor It puts, is also possible to obtain other drawings based on these drawings.
Fig. 1 is the flowage structure schematic diagram that the embodiment of the present invention prepares graphical sapphire substrate;
Wherein,
(1) the schematic diagram of the section structure of etch resistant coating and photoresist layer is formed for coating;
(2) the schematic diagram of the section structure for photoresist layer to be formed to mask pattern;
It (3) is the schematic diagram of the section structure that mask pattern is transferred to etch resistant coating;
It (4) is the schematic diagram of the section structure of removal photoresist;
(5) the graphical sapphire substrate pattern the schematic diagram of the section structure to be formed after etching Sapphire Substrate.
Appended drawing reference:
1- Sapphire Substrate;2- etch resistant coating;3- photoresist layer.
Specific embodiment
Technical solution of the present invention is clearly and completely described below in conjunction with the drawings and specific embodiments, but Be it will be understood to those of skill in the art that it is following described embodiments are some of the embodiments of the present invention, rather than it is whole Embodiment is merely to illustrate the present invention, and is not construed as limiting the scope of the invention.Based on the embodiments of the present invention, ability Domain those of ordinary skill every other embodiment obtained without making creative work, belongs to guarantor of the present invention The range of shield.The person that is not specified actual conditions in embodiment, carries out according to conventional conditions or manufacturer's recommended conditions.Agents useful for same Or production firm person is not specified in instrument, is the conventional products that can be obtained by commercially available purchase.
A kind of preparation method of graphical sapphire substrate, includes the following steps:
(a) it coats to form etch resistant coating in sapphire substrate surface;
(b) siliceous photoresist is coated in etch resistant coating surface and form siliceous photoresist layer, be lithographically formed mask pattern;
(c) etch resistant coating is etched under the protection of siliceous photoresist layer, and mask pattern is transferred to etch resistant coating;
(d) siliceous photoresist is removed;
(e) etch resistant coating and Sapphire Substrate are etched, the graphical sapphire substrate is obtained.
In a preferred embodiment of the invention, the silicone content of the siliceous photoresist is 30%-45%.It is furthermore preferred that The silicone content of the siliceous photoresist is 40%-42%.
Siliceous photoresist has good etch resistance energy, and is clearly distinguishable from the etching ratio of organic etch resistant coating, Therefore thickness control can meet the requirement of etch resistance energy in 100 nanometer level, and ultra-thin film thickness can be exposed using contact Light mode forms mask pattern, and avoiding common thick film photoresist, in contact exposure, existing resolution ratio is low, has standing wave effect It answers, the problem that poor contrast, figure consistency difference etc. cause yield low.
In an of the invention preferred embodiment, the photoresist layer with a thickness of 50-500nm.It is furthermore preferred that the light Photoresist layer with a thickness of 80-150nm.
In a preferred embodiment of the invention, the etch resistant coating is organic etch resistant material.Optional routine has Machine etch resistant material, etch resistant coating is without having photosensitive property, and light source is through light when can reduce exposure using one side Reflex after photoresist thin layer on a sapphire substrate;On the other hand, siliceous photoresist layer and Sapphire Substrate are avoided Directly there is etching selection ratio difference in contact, improve etching efficiency.It is furthermore preferred that organic etch resistant material includes Thermosetting resin.It is further preferred that organic etch resistant material further includes curing agent.
Corresponding curing agent is added in thermosetting resin, can be improved the curing rate of etch resistant material, guarantees solidification The compactness of product structure improves the etch resistance energy of etch resistant coating.
In an of the invention preferred embodiment, the etch resistant coating with a thickness of 1-3 μm.It is furthermore preferred that described resistance to Etch coating with a thickness of 1.5-2.5 μm.
In a preferred embodiment of the invention, in the step (b), is formed and covered on photoresist layer by yellow light technique Film pattern forms required light specifically, the siliceous photoresist is toasted by yellow light technique, exposed, developed Needle drawing shape.Preferably, Exposure mode can be using primary complete molding contact exposure, when avoiding existing projection exposure It needs to carry out subregion multistep scan exposure, complex process and time-consuming and there is have stitching error to easily cause pattern shape between visual field The problem of change.
In a preferred embodiment of the invention, by plasma etching etch resistant coating in the step (c), it will cover Film pattern is transferred to etch resistant coating.It is furthermore preferred that containing oxygen element in the plasma etching gas.Since etch resistant applies Layer main component is hydrocarbon oxygen organic compound, and photoetching offset plate figure layer main component is silicon and oxygen, therefore using routine Oxygen-containing etching gas can easily etch away the etch resistant coating not under the protection of photoetching offset plate figure layer.
In a preferred embodiment of the invention, siliceous photoresist is removed by plasma etching in the step (d) Layer.It is furthermore preferred that the plasma etching gas contains fluorine element.The silicon content of siliceous photoresist layer is about 40%, ingredient Already close to silica, photoresist layer can be etched away using conventional fluorine-containing etching gas atmosphere.
In a preferred embodiment of the invention, pass through sense coupling etch resistant in the step (e) Coating and Sapphire Substrate.It is furthermore preferred that the etching gas is Cl2And BCl3.Sense coupling is high-efficient, Etching injury is small, and uniformity is good, at low cost.By above-mentioned condition, the etching speed that ICP mode etches Sapphire Substrate can be improved Rate.
Embodiment 1
Illustrate the implementation process of the preparation method of graphical sapphire substrate of the present invention below by specific embodiment: Referring to Fig. 1, it is the flowage structure schematic diagram that the present embodiment prepares graphical sapphire substrate, wherein (1) formed for coating The schematic diagram of the section structure of etch resistant coating and photoresist layer;(2) cross-section structure for photoresist layer is formed mask pattern shows It is intended to;It (3) is the schematic diagram of the section structure that mask pattern is transferred to etch resistant coating;It (4) is the section knot of removal photoresist Structure schematic diagram;(5) the graphical sapphire substrate pattern the schematic diagram of the section structure to be formed after etching Sapphire Substrate.
The preparation method of graphical sapphire substrate described in the present embodiment, includes the following steps:
(a) it coats to form etch resistant coating 2 on 1 surface of Sapphire Substrate;Specifically,
(a1) 1 surface of Sapphire Substrate is subjected to purification pretreatment:
Sapphire Substrate 1 is placed in trichloroethanes, is cleaned by ultrasonic 10min, is subsequently placed in acetone, is cleaned by ultrasonic 2min;Ion Cleaning is spent, after the sulfuric acid and nitric acid dousing 10min for being then 1 ﹕ 1 with volume ratio, is cleaned with deionized water dry Only, it is dried to obtain the Sapphire Substrate 1 of purified treatment;
(a2) bimaleimide resin is coated by spin-coating method on 1 surface of Sapphire Substrate of above-mentioned purified processing BMI-1500 (production firm: Designer molecules company) after coating, solidifies in 210 DEG C of baking 2min, makes it Remove the etch resistant coating 2 for the even compact that solvent is formed with a thickness of 2 μm;
(b) siliceous photoresist is coated on 2 surface of etch resistant coating, forms photoresist layer 3, and be lithographically formed mask pattern; Specifically,
2 surface of etch resistant coating of above-mentioned formation by spin-coating method coat siliceous photoresist SUN-iHM (production firm: Weifang Xingtaike Microelectronic Materials Co., Ltd.), the front baking of 1min is carried out at 60 DEG C, removes solvent, is formed with a thickness of 100nm Photoresist layer 3;Using contact exposure machine at 365nm, photoresist layer is exposed with the light exposure of 60mj, is then existed The middle baking that 1min is carried out at 130 DEG C, develops in the TMAH aqueous solution that mass fraction is 2.38%, forms as shown in Fig. 1 (2) Structure;
(c) under the protection of photoresist, etch resistant coating is performed etching;It is specific:
Using oxygen as dry etching gas, organic etch resistant coating of unglazed photoresist protection portion point is etched away, is formed The structure as shown in Fig. 1 (3), so that mask pattern is transferred to etch resistant coating;
(d) photoresist layer is removed;It is specific:
Switch etching gas ingredient, using CF4As main etching gas, siliceous photoresist layer is performed etching, is removed Photoresist forms the structure as shown in Fig. 1 (4);
(e) etch resistant coating and Sapphire Substrate are etched, the graphical sapphire substrate is obtained;It is specific:
Switch etching gas ingredient again, uses mass flow ratio for the Cl of 1 ﹕ 42And BCl3, precious to etch resistant coating and indigo plant Stone lining bottom performs etching, and final etch resistant coating is all etched, and forms the structure as shown in Fig. 1 (5).
The structure of the graphical sapphire substrate is not limited to this, can adjust according to actual needs to mask pattern It is whole, and then obtain graphical sapphire substrate of different shapes.
Embodiment 2
The preparation method of the present embodiment reference implementation example 1, difference are only that the silicone content of the siliceous photoresist is 42%.
Embodiment 3
The preparation method of the present embodiment reference implementation example 1, difference are only that the silicone content of the siliceous photoresist is 40%.
Embodiment 4
The preparation method of the present embodiment reference implementation example 1, difference be only that, the photoresist layer with a thickness of 80nm.
Embodiment 5
The preparation method of the present embodiment reference implementation example 1, difference be only that, the photoresist layer with a thickness of 150nm.
The preparation method of the graphical sapphire substrate through the invention is applied using siliceous photoresist combination etch resistant Layer, increases etch resistance energy, the photoresist layer of ultrathin make can to meet using contact exposure mode technique to point The high request of resolution and yield, is effectively controlled equipment cost.Also, preparation method of the invention, can according to actual needs, Transfer mask figure obtains different targeted graphical Sapphire Substrate patterns, adaptable.
Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations;To the greatest extent Pipe present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: its according to So be possible to modify the technical solutions described in the foregoing embodiments, or to some or all of the technical features into Row equivalent replacement;And these are modified or replaceed, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution The range of scheme.

Claims (14)

1. a kind of preparation method of graphical sapphire substrate, which comprises the steps of:
(a) it coats to form etch resistant coating in sapphire substrate surface;
(b) siliceous photoresist is coated in etch resistant coating surface and form siliceous photoresist layer, using contact exposure mode photoetching Form mask pattern;
(c) etch resistant coating is etched under the protection of siliceous photoresist layer, and mask pattern is transferred to etch resistant coating;
(d) siliceous photoresist is removed;
(e) etch resistant coating and Sapphire Substrate are etched, the graphical sapphire substrate is obtained;
The material of the etch resistant coating is organic etch resistant material;Organic etch resistant material includes thermosetting resin;
Organic etch resistant material is coated on sapphire substrate surface, is heating and curing to form the etch resistant coating;
The silicone content of the siliceous photoresist is 30%-45%.
2. the preparation method of graphical sapphire substrate according to claim 1, which is characterized in that
The silicone content of the siliceous photoresist is 40%-42%.
3. the preparation method of graphical sapphire substrate according to claim 1, which is characterized in that
Organic etch resistant material further includes curing agent.
4. the preparation method of graphical sapphire substrate according to claim 1, which is characterized in that the photoresist layer With a thickness of 50-500nm.
5. the preparation method of graphical sapphire substrate according to claim 1, which is characterized in that the photoresist layer With a thickness of 80-150nm.
6. the preparation method of graphical sapphire substrate according to claim 1, which is characterized in that the etch resistant coating With a thickness of 1-3 μm.
7. the preparation method of graphical sapphire substrate according to claim 6, which is characterized in that the etch resistant coating With a thickness of 1.5-2.5 μm.
8. the preparation method of graphical sapphire substrate according to claim 1, which is characterized in that in the step (b), By baking, exposure and imaging, mask pattern is formed on photoresist layer.
9. the preparation method of graphical sapphire substrate according to claim 1, which is characterized in that in the step (c) By plasma etching etch resistant coating, mask pattern is transferred to etch resistant coating.
10. the preparation method of graphical sapphire substrate according to claim 9, which is characterized in that the step (c) In, contain oxygen element in the plasma etching gas.
11. the preparation method of graphical sapphire substrate according to claim 1, which is characterized in that in the step (d) Photoresist is removed by plasma etching.
12. the preparation method of graphical sapphire substrate according to claim 11, which is characterized in that the step (d) In, the plasma etching gas contains fluorine element.
13. the preparation method of graphical sapphire substrate according to claim 1, which is characterized in that in the step (e) Pass through sense coupling etch resistant coating and Sapphire Substrate.
14. the preparation method of graphical sapphire substrate according to claim 13, which is characterized in that it is described inductively Plasma etching gas is Cl2And BCl3
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CN110752148A (en) * 2019-09-03 2020-02-04 福建晶安光电有限公司 Method for manufacturing patterned sapphire substrate by using photosensitive polysiloxane
CN116344686A (en) * 2023-05-31 2023-06-27 季华实验室 Method for manufacturing full-color display panel, display panel and display device

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103597619A (en) * 2012-03-07 2014-02-19 株式会社爱发科 Method for manufacturing element
CN105261682A (en) * 2015-10-16 2016-01-20 山东元旭光电有限公司 Sapphire composite substrate and preparing method thereof
CN106959586A (en) * 2015-12-09 2017-07-18 三星电子株式会社 The method of photoetching compositions and manufacture patterned devices

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103597619A (en) * 2012-03-07 2014-02-19 株式会社爱发科 Method for manufacturing element
CN105261682A (en) * 2015-10-16 2016-01-20 山东元旭光电有限公司 Sapphire composite substrate and preparing method thereof
CN106959586A (en) * 2015-12-09 2017-07-18 三星电子株式会社 The method of photoetching compositions and manufacture patterned devices

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