KR100543859B1 - Pretreatment Method of Sapphire Substrate by Using Sulfuric Acid to Fabricate High Quality Thin Films - Google Patents
Pretreatment Method of Sapphire Substrate by Using Sulfuric Acid to Fabricate High Quality Thin Films Download PDFInfo
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- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 239000000758 substrate Substances 0.000 title claims abstract description 46
- 229910052594 sapphire Inorganic materials 0.000 title claims abstract description 31
- 239000010980 sapphire Substances 0.000 title claims abstract description 31
- 239000010409 thin film Substances 0.000 title abstract description 11
- 238000002203 pretreatment Methods 0.000 title description 6
- 238000000034 method Methods 0.000 claims abstract description 7
- 238000005530 etching Methods 0.000 claims description 13
- 230000003746 surface roughness Effects 0.000 abstract description 4
- 230000000052 comparative effect Effects 0.000 description 7
- 239000011259 mixed solution Substances 0.000 description 5
- 229910019142 PO4 Inorganic materials 0.000 description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 4
- 238000000089 atomic force micrograph Methods 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- 238000000151 deposition Methods 0.000 description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 4
- 239000010452 phosphate Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000012153 distilled water Substances 0.000 description 3
- 230000005693 optoelectronics Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000011282 treatment Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 229910002601 GaN Inorganic materials 0.000 description 2
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000005498 polishing Methods 0.000 description 2
- 239000011787 zinc oxide Substances 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000003486 chemical etching Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 238000004439 roughness measurement Methods 0.000 description 1
- 238000000427 thin-film deposition Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
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Abstract
본 발명은 고품질의 박막을 증착하기 위하여 황산 (H2SO4) 용액을 이용하여 사파이어 기판을 전처리하는 방법에 관한 것이다. 본 발명에 따를 경우 표면이 평탄하고 표면의 평균 조도 (surface RMS roughness)가 0.20 nm 이하로 매우 매끄러우며 피트 (pit)가 없는 우수한 표면을 갖는 기판을 얻을 수 있다. 또한, 이러한 기판을 이용하여 박막을 증착시 기판에 의한 영향을 최소화할 수 있다.The present invention relates to a method of pretreating a sapphire substrate using sulfuric acid (H 2 SO 4 ) solution to deposit a high quality thin film. According to the present invention, it is possible to obtain a substrate having an excellent surface with a flat surface and very smooth surface average surface roughness of 0.20 nm or less and no pit. In addition, it is possible to minimize the influence of the substrate when the thin film is deposited using such a substrate.
사파이어 기판, 황산, 피트, 평균 조도Sapphire Substrate, Sulfuric Acid, Feet, Average Roughness
Description
도 1은 320℃의 황산 중에서 30분간 에칭된 사파이어 기판 표면의 AFM 사진 (a) 및 160℃의 3:1 부피비 황산:인산 혼합 용액 중에서 10분간 에칭된 사파이어 기판 표면의 AFM 사진 (b).1 is an AFM image of a sapphire substrate surface etched for 30 minutes in sulfuric acid at 320 ° C. (a) and an AFM image of a sapphire substrate surface etched for 10 minutes in a 3: 1 volumetric sulfuric acid: phosphate mixed solution at 160 ° C. (b).
본 발명은 고품질의 박막을 증착하기 위하여 증착 전에 기판의 결함을 제거하기 위하여 행하는 화학적 기판 전처리 방법에 관한 것이다.The present invention relates to a chemical substrate pretreatment method which is performed to remove defects of a substrate before deposition in order to deposit a high quality thin film.
현재 발광 다이오드(LEDs), 레이저 다이오드(LDs) 및 자외선 검출기 등과 같은 광전자 부품으로의 응용을 위한 갈륨질화물, 아연산화물 등과 같은 III-V족 및 II-V족 박막의 수요가 급격히 증가해 왔으며, 이러한 고품질의 박막을 증착하기 위해서는 증착될 박막과 격자의 배열 및 상수가 유사하고 표면이 매끄러우며 결함이 없는 기판이 필요하다. 이와 같은 고품질의 박막을 증착하기 위해 일반적으로 사 용되는 기판은 사파이어(sapphire, α-Al2O3) 기판으로서, 위에 언급된 증착될 박막의 격자 상수와의 차이는 다소 존재하나 화학적 친화성, 광학적 투과성, 높은 온도 안정성 및 비교적 낮은 가격으로 인하여 널리 사용되고 있다.Currently, the demand for III-V and II-V thin films such as gallium nitride, zinc oxide, etc. for the application to optoelectronic components such as light emitting diodes (LEDs), laser diodes (LDs) and ultraviolet detectors has increased rapidly. Deposition of high quality thin films requires substrates with similar lattice arrangements and constants, smooth surfaces and free of defects. A substrate commonly used for depositing such high quality thin films is a sapphire (α-Al 2 O 3 ) substrate, which has a slight difference from the lattice constant of the thin film to be deposited as mentioned above, but with chemical affinity, It is widely used due to its optical transmission, high temperature stability and relatively low cost.
이러한 사파이어 기판은 그 표면을 평탄하고 매끄럽게 하기 위해 화학적-기계적 연마 처리되어 판매가 되나, 이러한 연마 처리는 기판 표면에 스크래치나 잔류 응력이 남게 하여 광전자 부품 연구자나 생산자가 박막 증착 전에 화학적으로 에칭하는 전처리 과정을 필요하게 한다. 이러한 화학적 에칭 전처리 방법 중 가장 널리 이용되는 화학적 전처리 방법은 3:1 부피비 황산(H2SO4):인산(H3PO 4) 혼합 용액에 사파이어 기판을 넣어 에칭하는 방법이나, 이 방법은 표면을 평탄하고 매끄럽게는 하나 증착될 박막의 광 특성을 저하시키는 원인이 되는, 표면을 움푹 들어가게 하는 피트 (pit)의 형성을 억제하지 못 한다는 문제점이 있다. 따라서, 평평하고 매끄러운 표면을 가지면서 피트가 없는 기판이 제공되는 전처리 방법이 요구되고 있다.These sapphire substrates are sold with chemical-mechanical polishing treatments to smooth and smooth their surfaces, but these polishing treatments leave scratches or residual stresses on the substrate surface, pretreatment process that the optoelectronic component researchers or producers chemically etch before thin film deposition. Makes it necessary. Among the chemical etching pretreatment methods, the most widely used chemical pretreatment method is to etch a sapphire substrate in a 3: 1 volume ratio sulfuric acid (H 2 SO 4 ): phosphate (H 3 PO 4 ) mixed solution, but this method There is a problem that flatness and smoothness, however, do not inhibit the formation of pits that dent the surface, which causes deterioration in the optical properties of the thin film to be deposited. Therefore, there is a need for a pretreatment method in which a substrate having a pit free and having a flat smooth surface is provided.
따라서, 본 발명의 목적은 매우 매끄러운 표면을 가지며 피트 및 스크래치 등의 결함이 없는 사파이어 기판이 제공되는 사파이어 기판의 전처리 방법을 제공하는 것이다.Accordingly, it is an object of the present invention to provide a method for pretreatment of a sapphire substrate which is provided with a sapphire substrate having a very smooth surface and free of defects such as pits and scratches.
본 발명자들은 황산(H2SO4)을 이용하여 사파이어 기판을 에칭하여 전처리할 경우 매우 매끄러운 표면을 가지며 피트 및 스크래치 등의 결함이 없는 사파이어 기판이 제공되는 것을 발견하여 본 발명에 이르렀다.The inventors have found that a sapphire substrate having a very smooth surface and free of defects such as pits and scratches is provided when the sapphire substrate is etched using sulfuric acid (H 2 SO 4 ) to be pretreated.
본 발명의 사파이어 기판의 전처리 방법은 황산에 사파이어 기판을 넣은 후 310 내지 330℃에서 20 내지 40분 동안 가열하여 사파이어 기판을 에칭하는 단계를 포함한다.The pretreatment method of the sapphire substrate of the present invention includes the step of etching the sapphire substrate by placing the sapphire substrate in sulfuric acid and then heating at 310 to 330 ° C. for 20 to 40 minutes.
본 발명에서 사용되는 황산은 순수한 황산을 사용하는 것이 바람직하나, 농도가 90％ 이상인 진한 황산도 사용가능하다.It is preferable to use pure sulfuric acid as the sulfuric acid used in the present invention, but concentrated sulfuric acid having a concentration of 90% or more can be used.
에칭 온도는 310 내지 330℃가 바람직하며, 에칭 온도가 310℃ 미만이거나 또는 330℃를 초과할 경우 얻어지는 사파이어 기판의 표면 평균 조도가 커지게 된다.The etching temperature is preferably 310 to 330 ° C, and the surface average roughness of the sapphire substrate obtained when the etching temperature is lower than 310 ° C or higher than 330 ° C becomes large.
또한, 에칭 시간은 20 내지 40분을 할 경우 가장 우수한 표면 평균 조도를 갖는 표면을 얻을 수 있다.In addition, when the etching time is 20 to 40 minutes, the surface having the best surface average roughness can be obtained.
이와 같은 황산 에칭 후의 기판 처리는 일반적으로 공지되어 있는 방법으로 처리할 수 있으며, 예를 들면, 황산 에칭 후 기판을 증류수에 담근 채로 초음파 세척기에서 10분간 세척한 후 질소 가스를 불어 기판의 표면에 있는 증류수를 제거한다.Such substrate treatment after sulfuric acid etching can be treated by a generally known method. For example, after sulfuric acid etching, the substrate is immersed in distilled water for 10 minutes in an ultrasonic cleaner, and then blown with nitrogen gas to the surface of the substrate. Remove distilled water.
이하, 본 발명을 실시예로써 더욱 자세히 설명하나, 본 발명은 하기 실시예에 의해 한정되는 것은 아니다.Hereinafter, the present invention will be described in more detail with reference to Examples, but the present invention is not limited by the following Examples.
<실시예 1><Example 1>
사파이어 기판 (Kyocera TS-3577)을 일반적인 유기물 세척 방법인 아세톤, 메탄올 및 증류수를 이용하여 세척한 후 건조하였다. 이와 같이 준비한 사파이어 기판 시료를 순수한 황산이 담긴 비이커에 넣은 후 PID 조절 기능이 있는 열판 (hot plate, 미성 MS100D) 위에서 각각 300℃, 310℃, 320℃, 330℃ 또는 350℃의 온도로 안전상 분당 10℃로 가열한 후 각 온도에서 30분 동안 에칭하였다. 이때, 황산 용액의 온도는 두개의 온도센서 (thermocouple)를 이용하여 측정하였는데, 하나는 황산 용액 중에, 다른 하나는 열판의 표면 하부에 위치시켜 정확한 온도를 보정하여 설정 온도에 비해 실제 용액의 온도가 1℃ 이내의 오차 범위에 있도록 하였다.The sapphire substrate (Kyocera TS-3577) was washed with acetone, methanol and distilled water, which are common organic material washing methods, and then dried. The sapphire substrate sample thus prepared is placed in a beaker containing pure sulfuric acid, and then on a hot plate with a PID control function (hot plate, micro MS100D) at a temperature of 300 ° C., 310 ° C., 320 ° C., 330 ° C. or 350 ° C., respectively. After heating to < RTI ID = 0.0 > C, < / RTI > At this time, the temperature of the sulfuric acid solution was measured by using two thermocouples, one of the sulfuric acid solution, and the other is located under the surface of the hot plate to correct the correct temperature so that the actual solution temperature compared to the set temperature It was to be in the error range within 1 degreeC.
이와 같이 황산 처리를 한 시료를 AFM (Atomic Force Microscope, PSI)을 이용하여 표면의 상태 및 표면의 평균 조도를 측정하였다. 도 1(a)에 320℃의 황산 중에서 30분간 에칭된 사파이어 기판 표면의 AFM 사진을 나타내었다. 표면의 평균 조도는 5 x 5㎛ 영역의 주사 (scan)를 통해 결정하였다.The sulfuric acid treated samples were measured using AFM (Atomic Force Microscope, PSI) to measure the state of the surface and the average roughness of the surface. 1 (a) shows an AFM image of the surface of a sapphire substrate etched in sulfuric acid at 320 ° C. for 30 minutes. The average roughness of the surface was determined by a scan of the 5 x 5 μm area.
<비교예 1>Comparative Example 1
실시예 1과 같이 사파이어 기판을 준비한 후, 이 기판을 3:1 부피비 황산(H2SO4):인산(H3PO4) 혼합 용액이 담긴 비이커에 넣은 후 PID 조절 기능이 있는 열판 위에서 160℃로 분당 10℃로 가열한 후 10분 동안 에칭하였다.After preparing a sapphire substrate as in Example 1, the substrate was placed in a beaker containing a 3: 1 volumetric sulfuric acid (H 2 SO 4 ): phosphate (H 3 PO 4 ) mixed solution and then 160 ° C. on a hot plate with PID control. Heated to 10 ° C. per minute and then etched for 10 minutes.
이와 같이 3:1 황산(H2SO4):인산(H3PO4) 혼합 용액 처리한 시료의 표면을 AFM을 이용하여 실시예 1과 같이 표면의 상태 및 표면의 평균 조도를 측정하였다. 도 1(b)에 사파이어 기판 표면의 AFM 사진을 나타내었다.As described in Example 1, the surface of the sample treated with the 3: 1 sulfuric acid (H 2 SO 4 ): phosphate (H 3 PO 4 ) mixed solution was measured using AFM, and the surface roughness and average roughness of the surface were measured. An AFM image of the surface of the sapphire substrate is shown in FIG.
상기 실시예 1 및 비교예 1에서 얻은 시료의 표면의 상태 및 표면의 평균 조도의 결과를 하기 표 1에 나타내었다.Table 1 shows the results of the surface roughness and average surface roughness of the samples obtained in Example 1 and Comparative Example 1.
상기 표 1로부터 알 수 있듯이, 3:1 부피비 황산(H2SO4):인산(H3PO4 ) 혼합 용액을 이용하여 160℃에서 10분간 전처리한 비교예 1의 사파이어 기판은 표면이 비교적 평탄하고 매끄러우나 기판 표면에 큰 피트들이 형성되어 있었다. 이에 반해, 순수한 황산을 이용하여 전처리한 본 발명에 따른 실시예 1의 사파이어 기판의 경우 표면이 평탄하고 매우 매끄러울 뿐만 아니라 피트가 없거나 거의 없는 우수한 표면을 가지고 있었다.As can be seen from Table 1, the sapphire substrate of Comparative Example 1 pretreated at 160 ° C. for 10 minutes using a 3: 1 volumetric sulfuric acid (H 2 SO 4 ): phosphoric acid (H 3 PO 4 ) mixed solution has a relatively flat surface. It was smooth, but large pits were formed on the surface of the substrate. In contrast, the sapphire substrate of Example 1 according to the present invention pretreated with pure sulfuric acid had an excellent surface having a smooth and very smooth surface as well as little or no pit.
또한, 표면의 평균 조도 측정값을 보면, 비교예 1의 사파이어 기판은 0.34 nm의 표면 평균 조도를 나타낸 데 반해, 본 발명에 따른 실시예 1의 사파이어 기판의 경우 310℃ 및 350℃의 에칭 온도에서는 비교예 1의 경우보다 다소 평균 조도가 컸으나, 에칭 온도 300 내지 330℃에서는 0.20 내지 0.16 nm로 비교예 1의 경우보다 우수함을 알 수 있었다.In addition, the average roughness measurement value of the surface shows that the sapphire substrate of Comparative Example 1 shows a surface average roughness of 0.34 nm, whereas in the case of the sapphire substrate of Example 1 according to the present invention, the etching temperature of 310 ° C and 350 ° C The average roughness was somewhat larger than that of Comparative Example 1, but 0.20 to 0.16 nm was found to be superior to that of Comparative Example 1 at an etching temperature of 300 to 330 ° C.
본 발명에 따라 사파이어 기판을 황산을 이용하여 전처리할 경우 평탄하고 매우 매끄러우며 피트가 없는 사파이어 기판을 얻을 수 있다. 또한, 본 발명에 따라 얻어지는 이러한 사파이어 기판을 이용하여 박막을 증착시 기판에 의한 영향을 최소화할 수 있어, 발광 다이오드 (LEDs), 레이저 다이오드 (LDs) 및 자외선 검출기 등과 같은 광전자 부품 제조시 갈륨질화물, 아연산화물과 같은 III-V족 및 II-VI족 박막의 특성을 향상시킬 수 있다.According to the present invention, when the sapphire substrate is pretreated with sulfuric acid, a sapphire substrate that is flat, very smooth, and without pits can be obtained. In addition, by using the sapphire substrate obtained in accordance with the present invention it is possible to minimize the influence of the substrate when depositing a thin film, gallium nitride in the production of optoelectronic components, such as light emitting diodes (LEDs), laser diodes (LDs) and ultraviolet detectors, It is possible to improve the properties of group III-V and II-VI thin films such as zinc oxide.
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