CN101788415B - Corroding agent for detecting damage of surface layer of sapphire substrate - Google Patents
Corroding agent for detecting damage of surface layer of sapphire substrate Download PDFInfo
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- CN101788415B CN101788415B CN2010101289538A CN201010128953A CN101788415B CN 101788415 B CN101788415 B CN 101788415B CN 2010101289538 A CN2010101289538 A CN 2010101289538A CN 201010128953 A CN201010128953 A CN 201010128953A CN 101788415 B CN101788415 B CN 101788415B
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- corroding
- acid
- sapphire substrate
- mordant
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Abstract
The invention belongs to the field of ultra-precision processing of hard and brittle crystal materials and relates to a corroding agent for detecting damage of a surface layer of a sapphire substrate. The corroding agent is formed by the mixing of thiocyanic acid (HCNS), concentrated sulfuric acid (H2SO4) and concentrated phosphoric acid (H3PO4). The volume percent of each component is as follows: the thiocyanic acid: 20 to 25%; the concentrated sulfuric acid: 55 to 60%; the concentrated phosphoric acid: 15 to 20%; and the total volume percent of each component is 100%. According to the needed volume of the corroding agent, the volume of the thiocyanic acid (HCNS), the concentrated sulfuric acid (H2SO4) and the concentrated phosphoric acid (H3PO4) is respectively measured according to the above proportion, and then the three components are uniformly stirred under normal temperature and pressure. The corroding agent has good preferential corroding property against the sapphire substrate and also has the characteristics of obvious damage corroding effect, low using temperature and high corroding speed.
Description
Technical field
The invention belongs to hard and brittle crystal materials ultraprecise manufacture field, relate to a kind of mordant that is used to detect damage of surface layer of sapphire substrate.
Background technology
Monocrystalline sapphire (Sapphire, α-Al
2O
3) be a kind of multi-functional crystalline material with good optical property, physical property and chemical property.Have characteristics such as hardness height (Mohs 9 is only second to the adamas that hardness is Mohs 10), fusing point height, light transmission good (infrared band substantially transparent), electrical insulating property excellence, stable chemical performance.Aspect optics, monocrystalline sapphire is used for the catoptron window of laser instrument, and simultaneously, it also is one of critical material of infrared guidance weapon.Aspect electronics, monocrystalline sapphire can be used as the semiconductor material of heteroepitaxial growth or the substrate of metal material, as is used for epitaxial substrate material of GaN light emitting diode (LED) etc.
No matter sapphire substrate still is the substrate of microelectronic as the window in optical communication field, all its machined surface layer quality is had very high requirement, and the superficial layer quality of substrate directly influences the important indicators such as usability, yield rate and life-span of device.Need a series of machinery and chiral process from the sapphire single-crystal ingot to sapphire substrate, as cutting, grinding, polishing etc., inevitably can produce machining damages such as little cut, little spots, unrelieved stress, distortion of lattice on substrate surface/surface, Asia, these machining damages can influence the physicochemical property and the usability of finished surface, therefore, the damage of surface layer of sapphire substrate is an important indicator weighing the substrate crudy.At present, the main distribution of adopting preferential etching microscopic observation method to detect surface damages such as sapphire substrate surface scratch, micro-crack, pit, orange peel adopts cross section microscopic observation method and angle polishing microscopic observation method to detect feature, the degree of depth and the regularity of distribution etc. of sapphire substrate sub-surface damage.The detection principle of preferential etching microscopic observation method, cross section microscopic observation method and angle polishing microscopic observation method is that the local stress field that the damage of substrate surface layer causes promotes the chemical corrosion rate of damage location to accelerate, cause the chemical corrosion rate at damage location and not damaged position difference to occur, promptly can be observed damage of surface layer of sapphire substrate position and the contrast of not damaged position formation light and shade at microscopically.Therefore, the damage of surface layer that adopts said method to detect sapphire substrate must select suitable chemical mordant corrosion to detect the position, but existing chemical mordant such as molten sodium hydroxide (NaOH), molten potassium hydroxide (KOH), the concentrated sulphuric acid (H
2SO
4), sodium borate glass metal (Na
2O-B
2O
3) wait and in corrosion process, exist etching time long, require shortcomings such as the high and repeatable difference of corrosion temperature.Therefore, the chemical mordant of the new prescription of research is the convenient key that accurately detects damage of surface layer of sapphire substrate, and is significant for the surface working that guarantees sapphire substrate.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of mordant that is used to detect damage of surface layer of sapphire substrate, it is slow to solve the speed that present mordant exists in substrate surface/sub-surface damage corrosion process, the serviceability temperature height, shortcomings such as corrosive effect and poor repeatability.
The technical solution used in the present invention is a kind of mordant that is used to detect damage of surface layer of sapphire substrate, it is characterized in that, mordant is by thiocyanic acid (HCNS), the concentrated sulphuric acid (H
2SO
4) and strong phosphoric acid (H
3PO
4) form, the shared percent by volume of each composition is: thiocyanic acid (HCNS) is 20-25%; The concentrated sulphuric acid (H
2SO
4) be 55-60%; Strong phosphoric acid (H
3PO
4) be 15-20%; Each composition percent by volume sum is 100%.Mordant volume according to using needs measures thiocyanic acid (HCNS) respectively, the concentrated sulphuric acid (H according to the above ratio
2SO
4) and strong phosphoric acid (H
3PO
4) volume, stirring under normal temperature, normal pressure then gets final product.
The present invention has following obvious effects:
1. mordant of the present invention has extraordinary preferential etch to sapphire substrate, and the substrate surface layer damage after the corrosion can clearly show under optical microscope.
2. the serviceability temperature of mordant of the present invention is low, only need remain on more than 150 ℃.
3. the corrosion rate of mordant of the present invention is fast, and corrosion process only needs 5min～6min.
Embodiment
The combination technology scheme is further described mordant of the present invention and embodiment thereof: mordant comprises: thiocyanic acid (HCNS), the concentrated sulphuric acid (H
2SO
4) and strong phosphoric acid (H
3PO
4).The mixing placement of each composition of mordant is followed successively by in proper order: HCNS → H
2SO
4→ H
3PO
4, stirring at normal temperatures and pressures gets final product.
Embodiment 1:
The sapphire substrate that the sample that is corroded polishes for the W0.5 diamond abrasive adopts preferential etching microscopic observation method to detect the degree of impairment on polishing substrate surface.According to the size of corrosion sample, the mordant volume of selection is 50ml, and each composition volume proportion is HCNS: H
2SO
4: H
3PO
4=10ml: 30ml: 10ml (20%: 60%: 20%), use spirit lamp heating mordant, keep the mordant temperature more than 150 ℃, then substrate is immersed in the mordant fully and take out behind 5min～6min, at last, use deionized water that the mordant of substrate surface is cleaned up and dry up substrate surface with high pressure air rifle.The substrate surface that adopts optical microscope promptly to can observe the processing of W0.5 diamond abrasive has tangible pit and scratch defects.
Embodiment 2:
The sample that is corroded is the sapphire substrate of #325 diamond wheel grinding, adopts cross section microscopic observation method to detect the degree of impairment on the inferior surface of grinding substrate.According to the size of corrosion sample, the mordant volume of selection is 20ml, and each composition volume proportion is HCNS: H
2SO
4: H
3PO
4=4ml: 12ml: 4ml (20%: 60%: 20%), use spirit lamp heating mordant, keep the mordant temperature more than 150 ℃, then substrate is immersed in the mordant fully and take out behind 5min～6min, at last, use deionized water that the mordant of substrate surface is cleaned up and dry up substrate surface with high pressure air rifle.The inferior surface of adopting optical microscope promptly to can observe #325 diamond wheel grinding substrate has the dislocation affected layer about 20 μ m.
Claims (1)
1. a mordant that is used to detect damage of surface layer of sapphire substrate is characterized in that, it is by thiocyanic acid (HCNS), the concentrated sulphuric acid (H
2SO
4) and strong phosphoric acid (H
3PO
4) mix, the shared percent by volume of each composition is: HCNS accounts for 20-25%, H
2SO
4Account for 55-60%, H
3PO
4Account for 15-20%, the summation of each composition percent by volume is 100%; Mordant volume according to using needs measures thiocyanic acid (HCNS) respectively, the concentrated sulphuric acid (H according to the above ratio
2SO
4) and strong phosphoric acid (H
3PO
4) volume, under normal temperature, normal pressure, mordant is stirred.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101289538A CN101788415B (en) | 2010-03-17 | 2010-03-17 | Corroding agent for detecting damage of surface layer of sapphire substrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101289538A CN101788415B (en) | 2010-03-17 | 2010-03-17 | Corroding agent for detecting damage of surface layer of sapphire substrate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101788415A CN101788415A (en) | 2010-07-28 |
| CN101788415B true CN101788415B (en) | 2011-09-14 |
Family
ID=42531711
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010101289538A Expired - Fee Related CN101788415B (en) | 2010-03-17 | 2010-03-17 | Corroding agent for detecting damage of surface layer of sapphire substrate |
Country Status (1)
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|---|---|
| CN (1) | CN101788415B (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102166790A (en) * | 2011-01-21 | 2011-08-31 | 苏州辰轩光电科技有限公司 | Processing method for removing rough surface and scars of sapphire substrate |
| CN102445373A (en) * | 2011-11-19 | 2012-05-09 | 元亮科技有限公司 | Detection method of sapphire monocrystal dislocation density |
| CN103645078B (en) * | 2013-12-05 | 2016-01-20 | 广东工业大学 | A kind of cross section quick Fabrication of single crystal semiconductor substrate and sub-crizzle detection method |
| CN104880459B (en) * | 2015-05-15 | 2017-09-26 | 哈尔滨飞机工业集团有限责任公司 | A kind of plane aluminium alloy skin-surface scratches detection method |
| CN107201518A (en) * | 2017-05-04 | 2017-09-26 | 中国第汽车股份有限公司 | A kind of coat of metal corrosive liquid |
| CN108318346B (en) * | 2018-04-25 | 2024-02-02 | 中国石油大学(北京) | Borehole collapse pressure testing device |
| CN111829941A (en) * | 2020-05-27 | 2020-10-27 | 盐城工学院 | Corrosive liquid for detecting gallium oxide single crystal processing surface damage layer and detection method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1833816A (en) * | 2005-11-23 | 2006-09-20 | 周海 | Nano-glass supersmooth processing technique of sapphire crystal sheet |
| CN101082550A (en) * | 2007-07-13 | 2007-12-05 | 浙江大学 | Etching liquid used for displaying silicon crystal material defect and method of use thereof |
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2010
- 2010-03-17 CN CN2010101289538A patent/CN101788415B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1833816A (en) * | 2005-11-23 | 2006-09-20 | 周海 | Nano-glass supersmooth processing technique of sapphire crystal sheet |
| CN101082550A (en) * | 2007-07-13 | 2007-12-05 | 浙江大学 | Etching liquid used for displaying silicon crystal material defect and method of use thereof |
Non-Patent Citations (2)
| Title |
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| 周海等.蓝宝石衬底片精密加工工艺研究.《现代制造工程》.2001,(第9期),13-14页. * |
| 王银珍等.表面处理对蓝宝石衬底的影响.《人工晶体学报》.2005,第34卷(第3期),第432页第1段. * |
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|---|---|
| CN101788415A (en) | 2010-07-28 |
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