CN105177718A - Six-edge pyramid graphical sapphire preparation method - Google Patents
Six-edge pyramid graphical sapphire preparation method Download PDFInfo
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- CN105177718A CN105177718A CN201510354323.5A CN201510354323A CN105177718A CN 105177718 A CN105177718 A CN 105177718A CN 201510354323 A CN201510354323 A CN 201510354323A CN 105177718 A CN105177718 A CN 105177718A
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Abstract
The invention provides a six-edge pyramid graphical sapphire preparation method, and relates to a sapphire preparation method. In the prior art, the six-edge pyramid is difficultly produced on the sapphire surface through the dry etching. A purpose of the present invention is to solve the problem in the prior art. The method comprises: placing a pre-treated conical graphical sapphire sheet into a quartz baskets, carrying out high temperature wet etching in a mixing solution A in a quartz beaker, rinsing the conical graphical sapphire sheet with deionized water, and carrying out blow-drying with nitrogen so as to obtain the six-edge pyramid graphical sapphire. According to the present invention, with the six-edge pyramid graphical sapphire preparation method, the conical graphical sapphire can be effectively converted into the six-edge pyramid graphical sapphire, the generated six-edge pyramid graphical sapphire is ordered and regular, the repeatability is good, the used device is simple, the operation is easy and is easy to master, and the process is safe and pollution-free. The present invention belongs to the field of sapphire preparation.
Description
Technical field
The present invention relates to a kind of sapphire preparation method.
Background technology
Sapphire single-crystal has the physical and chemical performance of many uniquenesses, important electronics, pottery, catalysis oxide material, in such applications, sapphire is as the substrate material needed for preparation GaN base thin film epitaxial growth, the GaN of growth in common Sapphire Substrate, a large amount of dislocation defects is upwards propagated from bottom.The GaN of growth in groove-shaped Sapphire Substrate (degree of depth 1 μm), GaN layer carries out lateral growth at Sapphire Substrate top, and pattern side wall defines during two growth front boundary mergences some cavities.The lateral growth region dislocation of the heterojunction structure of GaN on PSS has bent 90 °, and dislocation does not propagate into the surface of GaN layer, thus strengthens the luminescent properties of GaN base photodiode (LED).
The patterned substrate making method of sapphire single-crystal is mainly divided into dry etching and wet etching, current wet etching cost is lower, and easily obtain the figure with scarp at sapphire surface, dry etching is easily to sapphire substrate surface, particularly mesa edge position, causes certain pollution and damage, and wherein partial dislocation will extend in upper layer side epitaxial layers, be unfavorable for the further raising of epitaxial film film quality, also can not prepare hexagon pyramid at sapphire surface.
Summary of the invention
The object of the invention is, in order to solve the problem being dry-etched in sapphire surface and being difficult to make hexagon pyramid, to provide a kind of preparation method of hexagon pyramid graphic sapphire
The preparation method of hexagon pyramid graphic sapphire is realized by following steps:
One, pre-treatment: at room temperature, is placed in ethanol and soaks 10 ~ 15h by conical graphic sapphire sheet, then use the conical graphic sapphire sheet of deionized water rinsing, then nitrogen dries up;
Two, the conical graphic sapphire sheet after processing through step one is placed in the quartzy gaily decorated basket, mixed solution A in quartz beaker is warming up to 235 ~ 275 DEG C, wherein mixed solution A is the mixed solution of hydrogen peroxide, phosphoric acid and sulfuric acid, wherein the volume ratio of phosphoric acid and sulfuric acid is 1: (0.8 ~ 3.2), the quartzy gaily decorated basket being loaded with conical graphic sapphire sheet is put into quartz beaker, etching 8 ~ 25min;
Three, the graphic sapphire sheet after step 2 process is taken out from quartz beaker, then use the conical graphic sapphire sheet of deionized water rinsing, then nitrogen dries up, and obtains hexagon pyramid graphic sapphire.
In step 2, the volume ratio of hydrogen peroxide and sulfuric acid is 0 ~ 1: 100.
The container adopted in each step of the preparation method of hexagon pyramid graphic sapphire of the present invention can not react with the solution used.Such as adopt high purity quartz container.
The sulfuric acid used in step 2 of the present invention, hydrogen peroxide, phosphoric acid are commercially available prod.
The quartz products used in step one of the present invention to step 3, is U.S.'s GE quartz material and makes.
Conical graphic sapphire can be converted into hexagon pyramid graphic sapphire by the preparation method of hexagon pyramid graphic sapphire of the present invention effectively, and the hexagon pyramid graphic sapphire generated is regular, reproducible.The wet equipment adopted is simple, easy to operate, is easy to grasp, process safety, pollution-free.
The invention has the beneficial effects as follows:
(1) for the Stability Analysis of Structures of sapphire single-crystal, be difficult to etching and destroy the features such as covalent linkage, the present invention determines order and the material proportioning of wet etching solvent for use, adopts lithographic method of the present invention can obtain the orderly hexagon pyramid graphic sapphire in surface.
(2) carry out pre-treatment (step one) to conical graphic sapphire, utilize sapphire single-crystal immersion treatment in dehydrated alcohol, what this step was removed is mainly the pollutent more weak with surface bonding.Deionized water rinsing, nitrogen dries up, and prevents from sapphire sheet stays water stain.
(3) quartz container used in step 2 and step 3 has specific function structure.
(4) utilize the severe corrosive of sulfuric acid and phosphoric acid in step 2, go to destroy sapphire covalent linkage, different crystal face is carried out to the etching of different rates, thus etch hexagon pyramid figure at sapphire surface.
(5) adopt the mixing solutions heat treated of hydrogen peroxide, sulfuric acid and phosphoric acid in step 3, effectively can increase the etch rate of sapphire surface.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope diagram to the conical graphic sapphire processed without experiment one;
Fig. 2 is the scanning electron microscope diagram to the conical graphic sapphire processed without experiment one;
Fig. 3, be the scanning electron microscope diagram of the hexagon pyramid graphic sapphire of experiment one gained;
Fig. 4 is the scanning electron microscope diagram of the hexagon pyramid graphic sapphire of experiment one gained.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: the preparation method of present embodiment hexagon pyramid graphic sapphire is realized by following steps:
One, pre-treatment: at room temperature, is placed in ethanol and soaks 10 ~ 15h by conical graphic sapphire sheet, then use the conical graphic sapphire sheet of deionized water rinsing, then nitrogen dries up;
Two, the conical graphic sapphire sheet after processing through step one is placed in the quartzy gaily decorated basket, mixed solution A in quartz beaker is warming up to 235 ~ 275 DEG C, wherein mixed solution A is the mixed solution of hydrogen peroxide, phosphoric acid and sulfuric acid, wherein the volume ratio of phosphoric acid and sulfuric acid is 1: (0.8 ~ 3.2), the quartzy gaily decorated basket being loaded with conical graphic sapphire sheet is put into quartz beaker, etching 8 ~ 25min;
Three, the graphic sapphire sheet after step 2 process is taken out from quartz beaker, then use the conical graphic sapphire sheet of deionized water rinsing, then nitrogen dries up, and obtains hexagon pyramid graphic sapphire.
The vitriol oil in present embodiment step 2 and hydrogen peroxide are commercially available prod, and the mass percentage concentration of the vitriol oil is 98%, hydrogen peroxide to be mass percentage concentration be 30% commercially available hydrogen peroxide, phosphoric acid to be mass percentage concentration be 85% commercially available hydrogen peroxide.
The preparation method of present embodiment corner cone graphic sapphire is wet etching method, effectively conical graphic sapphire can be converted into hexagon pyramid graphic sapphire, and the hexagon pyramid graphic sapphire generated is regular, reproducible.The equipment that wet etching adopts is simple, easy to operate, is easy to grasp, process safety, pollution-free.
Embodiment two: present embodiment and embodiment one are 0 ~ 1: 100 unlike the volume ratio of hydrogen peroxide in step 2 and sulfuric acid.Other is identical with embodiment one.
Embodiment three: mixed solution A in quartz beaker is warming up to 240 ~ 270 DEG C unlike in step 2 by present embodiment and embodiment one or two.Other is identical with embodiment one or two.
Embodiment four: mixed solution A in quartz beaker is warming up to 245 ~ 265 DEG C unlike in step 2 by one of present embodiment and embodiment one to three.Other is identical with one of embodiment one to three.
Embodiment five: mixed solution A in quartz beaker is warming up to 250 ~ 260 DEG C unlike in step 2 by one of present embodiment and embodiment one to four.Other is identical with one of embodiment one to four.
Embodiment six: mixed solution A in quartz beaker is warming up to 235 DEG C unlike in step 2 by one of present embodiment and embodiment one to five.Other is identical with one of embodiment one to five.
Embodiment seven: one of present embodiment and embodiment one to six are 1: 1 unlike the volume ratio of phosphoric acid in mixed solution A in step 2 and sulfuric acid.Other is identical with one of embodiment one to six.
Embodiment eight: one of present embodiment and embodiment one to six put into quartz beaker unlike the quartzy gaily decorated basket of graphic sapphire sheet conical in step 2, etching 23min.Other is identical with one of embodiment one to six.
Test as follows, verify beneficial effect of the present invention:
Experiment one: the preparation method of hexagon pyramid graphic sapphire, it is realized by following steps:
One, pre-treatment: at room temperature, is placed in ethanol by conical graphic sapphire sheet and soaks 12h, then use the conical graphic sapphire sheet of deionized water rinsing, then nitrogen dries up;
Two, the conical graphic sapphire sheet after processing through step one is placed in the quartzy gaily decorated basket, mixed solution A in quartz beaker is warming up to 240 DEG C, wherein mixed solution A is Trace Hydrogen Peroxide, phosphoric acid and sulfuric acid mixture liquid, the volume ratio of phosphoric acid and sulfuric acid is 1: 1, in step 2, the volume ratio of hydrogen peroxide and sulfuric acid is 1: 100, the quartzy gaily decorated basket being loaded with conical graphic sapphire sheet is put into quartz beaker, high temperature wet etching 23min;
Three, the graphic sapphire sheet temperature after step 2 process is taken out from quartz beaker, then use the conical graphic sapphire sheet of deionized water rinsing, then nitrogen dries up;
Test the vitriol oil in a step 2 and hydrogen peroxide is commercially available prod, the mass percentage concentration of the vitriol oil is 98%, hydrogen peroxide to be mass percentage concentration be 30% commercially available hydrogen peroxide, phosphoric acid to be mass percentage concentration be 85% commercially available hydrogen peroxide.
The step one of experiment one all adopts U.S. GE quartz material instrument to step 3.
Carry out scanning electronic microscope (SEM) test to the conical graphic sapphire (Fig. 1, Fig. 2) processed without experiment one and the hexagon pyramid graphic sapphire (Fig. 3, Fig. 4) obtained after testing a process, the SEM spectrogram that test obtains is respectively as shown in Figure 1, Figure 2 with shown in Fig. 3, Fig. 4.From Fig. 3, Fig. 4, the hexagon pyramid graphic sapphire of generation is regular, reproducible.
Visible, the hexagon pyramid graphic sapphire through testing a generation is regular, reproducible, and the equipment adopted is simple, easy to operate, is easy to grasp, process safety, pollution-free.
Claims (8)
1. the preparation method of hexagon pyramid graphic sapphire, is characterized in that the preparation method of hexagon pyramid graphic sapphire is realized by following steps:
One, pre-treatment: at room temperature, is placed in ethanol and soaks 10 ~ 15h by conical graphic sapphire sheet, then use the conical graphic sapphire sheet of deionized water rinsing, then nitrogen dries up;
Two, the conical graphic sapphire sheet after processing through step one is placed in the quartzy gaily decorated basket, mixed solution A in quartz beaker is warming up to 235 ~ 275 DEG C, wherein mixed solution A is the mixed solution of hydrogen peroxide, phosphoric acid and sulfuric acid, wherein the volume ratio of phosphoric acid and sulfuric acid is 1: (0.8 ~ 3.2), the quartzy gaily decorated basket being loaded with conical graphic sapphire sheet is put into quartz beaker, etching 8 ~ 25min;
Three, the graphic sapphire sheet after step 2 process is taken out from quartz beaker, then use the conical graphic sapphire sheet of deionized water rinsing, then nitrogen dries up, and obtains hexagon pyramid graphic sapphire.
2. the preparation method of hexagon pyramid graphic sapphire according to claim 1, is characterized in that the volume ratio of hydrogen peroxide and sulfuric acid in step 2 is 0 ~ 1: 100.
3. the preparation method of hexagon pyramid graphic sapphire according to claim 1 and 2, is characterized in that, in step 2, mixed solution A in quartz beaker is warming up to 240 ~ 270 DEG C.
4. the preparation method of hexagon pyramid graphic sapphire according to claim 1 and 2, is characterized in that, in step 2, mixed solution A in quartz beaker is warming up to 245 ~ 265 DEG C.
5. the preparation method of hexagon pyramid graphic sapphire according to claim 1 and 2, is characterized in that, in step 2, mixed solution A in quartz beaker is warming up to 250 ~ 260 DEG C.
6. the preparation method of hexagon pyramid graphic sapphire according to claim 1 and 2, is characterized in that, in step 2, mixed solution A in quartz beaker is warming up to 235 DEG C.
7. the preparation method of hexagon pyramid graphic sapphire according to claim 1 and 2, is characterized in that the volume ratio of phosphoric acid and sulfuric acid in mixed solution A in step 2 is 1: 1.
8. the preparation method of hexagon pyramid graphic sapphire according to claim 1 and 2, is characterized in that quartz beaker put into by the quartzy gaily decorated basket of conical graphic sapphire sheet in step 2, etching 23min.
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| CN201510354323.5A CN105177718B (en) | 2015-06-24 | 2015-06-24 | The preparation method of six corner cone graphic sapphires |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105420816A (en) * | 2015-12-24 | 2016-03-23 | 哈尔滨工业大学 | Preparation method of graphical sapphire in shape of symmetric hexangular star |
| CN105552177A (en) * | 2015-12-24 | 2016-05-04 | 哈尔滨工业大学 | Preparation method for zero-gap triangular cone patterned sapphire |
| CN112701198A (en) * | 2020-12-25 | 2021-04-23 | 福建晶安光电有限公司 | Patterned substrate, light-emitting diode and preparation method |
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| CN101582479A (en) * | 2009-06-10 | 2009-11-18 | 上海蓝光科技有限公司 | Light emitting diode chip structure and manufacturing method thereof |
| CN103311097A (en) * | 2013-05-24 | 2013-09-18 | 中国科学院半导体研究所 | Method for manufacturing micro-nano graph on sapphire substrate |
| CN103887166A (en) * | 2014-03-18 | 2014-06-25 | 西安神光安瑞光电科技有限公司 | Method for preparing oxide substitutional patterned substrate |
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| CN101582479A (en) * | 2009-06-10 | 2009-11-18 | 上海蓝光科技有限公司 | Light emitting diode chip structure and manufacturing method thereof |
| CN103311097A (en) * | 2013-05-24 | 2013-09-18 | 中国科学院半导体研究所 | Method for manufacturing micro-nano graph on sapphire substrate |
| CN103887166A (en) * | 2014-03-18 | 2014-06-25 | 西安神光安瑞光电科技有限公司 | Method for preparing oxide substitutional patterned substrate |
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| 江忠永等: "干法和湿法图形化蓝宝石衬底在GaN基LED上的应用", 《2012（杭州）中国长三角照明科技论坛论文集》 * |
Cited By (3)
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|---|---|---|---|---|
| CN105420816A (en) * | 2015-12-24 | 2016-03-23 | 哈尔滨工业大学 | Preparation method of graphical sapphire in shape of symmetric hexangular star |
| CN105552177A (en) * | 2015-12-24 | 2016-05-04 | 哈尔滨工业大学 | Preparation method for zero-gap triangular cone patterned sapphire |
| CN112701198A (en) * | 2020-12-25 | 2021-04-23 | 福建晶安光电有限公司 | Patterned substrate, light-emitting diode and preparation method |
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| CN105177718B (en) | 2018-07-03 |
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