Xây dựng quy trình định lượng Cephalexin trong dược phẩm bằng phương pháp quang phổ UV - VIS
Quang phổ Laser
description
Transcript of Quang phổ Laser
![Page 1: Quang phổ Laser](https://reader035.fdocuments.net/reader035/viewer/2022062222/568159df550346895dc729dd/html5/thumbnails/1.jpg)
Quang phổ Laser
DÙNG PHỔ RAMAN VÀ PHỔ QUANG PHÁT QUANG
NGHIÊN CỨU ẢNH HƯỞNG CỦA TỈ LỆ KHÍ OXY VÀ SỰ Ủ NHIỆT ĐỐI VỚI
MÀNG TIO2 CHẾ TẠO BẰNG PP PHÚN XẠ MAGNETON PHẢN ỨNG
![Page 2: Quang phổ Laser](https://reader035.fdocuments.net/reader035/viewer/2022062222/568159df550346895dc729dd/html5/thumbnails/2.jpg)
![Page 3: Quang phổ Laser](https://reader035.fdocuments.net/reader035/viewer/2022062222/568159df550346895dc729dd/html5/thumbnails/3.jpg)
Quang phổ Laser
MỤC ĐÍCH:
Nghiên cứu sự ảnh hưởng của tỉ lệ dòng oxy đưa vào trong hệ phún xạ trong việc chế tạo màng
Nghiên cứu sự ảnh hưởng của nhiệt độ ủ trong quá trình hình thành cấu trúc của màng
![Page 4: Quang phổ Laser](https://reader035.fdocuments.net/reader035/viewer/2022062222/568159df550346895dc729dd/html5/thumbnails/4.jpg)
Quang phổ Laser
GiỚI THIỆU:
Chế tạo màng TiOx bằng phương pháp phún xạ magneton trực tiếp ở nhiệt độ phòng với tỉ lệ dòng oxy đưa vào khoảng 3-15%
Sau đó đem ủ nhiệt ở 350-750oC
Dùng phổ nhiễu xạ tia X, quang phát quang và phổ Raman để nghiên cứu tính chất của màng
2
22
FOFO % 100%
FO FAr
![Page 5: Quang phổ Laser](https://reader035.fdocuments.net/reader035/viewer/2022062222/568159df550346895dc729dd/html5/thumbnails/5.jpg)
Quang phổ Laser
THÍ NGHIỆM:
Dùng đế p-Si(100), làm sạch bởi H2SO4 và H2O
Target Ti tinh khiết 99.99%, đường kính 2in và được áp vào nguồn DC 100W
Đế được áp điện thế -150V
Khoảng cách giữa đế và bia là 100mm
Áp suất nền 2.7*10-4 Pa, Áp suất làm việc 2.7*10-4 Pa
Thời gian phún xạ 40 phút
Độ dày của màng từ 50-200nm
![Page 6: Quang phổ Laser](https://reader035.fdocuments.net/reader035/viewer/2022062222/568159df550346895dc729dd/html5/thumbnails/6.jpg)
Quang phổ Laser
Cấu trúc màng, thông tin phase (anatase hay rutile) đo bởi quang phổ kế tia X sử dụng bức xạ Cu Kα (0.1542nm). Made in Japan
Các liên kết được đo bởi phổ Raman. Made in France
Phổ PL dùng laser He-Cd 325nm 50mW, cách tử và CCD
ĐO TÍNH CHẤT MÀNG:
![Page 7: Quang phổ Laser](https://reader035.fdocuments.net/reader035/viewer/2022062222/568159df550346895dc729dd/html5/thumbnails/7.jpg)
Quang phổ Lazer
LabRAM HR UV/Vis/NIR
+ Ar ion CW Laser (514.5nm, 488nm) upto 40mW at sample.+ He-Cd CW Laser (325nm) -Auto motor controlled XY mapping stage
Anatase Rutile
![Page 8: Quang phổ Laser](https://reader035.fdocuments.net/reader035/viewer/2022062222/568159df550346895dc729dd/html5/thumbnails/8.jpg)
Quang phổ Laser
Anatase
APPLICATION 1- Paints, and Coating , emulsion interior Paints, Enamels 2- Road-Marking Paints 3- Filler , Primers, and undercoat 4- Paper Industry 5- Plastic Industry 6- Rubber Industry 7- Cement Industry.
widely used in painting, printing oilpaper makingPlasticRubberartificial fiber (sợi quang nhân tạo)welding electric (hàn điện)Enamel (tráng men)electric appliances and construction material etc
Rutile
![Page 9: Quang phổ Laser](https://reader035.fdocuments.net/reader035/viewer/2022062222/568159df550346895dc729dd/html5/thumbnails/9.jpg)
GIXRD patterns of titanium oxide films formed at: 3, 6, 10 and 15 FO2% and post-annealing at 750 °C for 2 min in air
RESULTS AND DISCUSSION_ The deposition time was fixed at 40 min.
_ The crystalline (101) anatase peak denoted as A(101) at 25,3°._ The (110) rutile peak denoted as R(110) at 27.4° can be easily observed from the TiOx thin film formed at 3 FO2%._ The intensity of anatase peaks at 3 FO2% is stronger than rutile peaks.
_ As FO2% is higher than 6%, the rutile peaks cannot be detected.
![Page 10: Quang phổ Laser](https://reader035.fdocuments.net/reader035/viewer/2022062222/568159df550346895dc729dd/html5/thumbnails/10.jpg)
GIXRD patterns of titanium oxide films formed at: 3 FO2% and post-annealed at RT, 350°C , 550°C , and 750°C for 2 min in air.
RESULTS AND DISCUSSION
_ TiOx film annealed at 350°C is still an amorphous film because of no distinct diffraction peak.
_ The mixed crystalline anatase and rutile films are obtained after 550°C and 750°C annealing.
_ The intensity of both anatase and rutile peaks increases with increasing temperature.
![Page 11: Quang phổ Laser](https://reader035.fdocuments.net/reader035/viewer/2022062222/568159df550346895dc729dd/html5/thumbnails/11.jpg)
Raman spectra of titanium oxide films formed at 3, 6, 10 and 15 FO2% and post-annealed at 750 °C for 2 min in air.
RESULTS AND DISCUSSION
_ The film at 3 FO2% shows several anatase peaks at 396 and 639 cm−1 and rutile peaks at 449 and 612 cm−1.
_ The rutile peaks decrease with increasing oxygen flow ratio.
_ The intensity of anatasepeak decreaseswith increasing oxygen flow ratio due to the reduction of film thickness.
![Page 12: Quang phổ Laser](https://reader035.fdocuments.net/reader035/viewer/2022062222/568159df550346895dc729dd/html5/thumbnails/12.jpg)
Raman spectra of titaniumoxide films at 3 FO2% and post-annealed at RT, 350 °C , 550 °C , and 750 °C for 2 min in air.
RESULTS AND DISCUSSION
_ The intensity of anatase peaks at 396 and 639 cm−1 and rutile peaks at 449 and612cm−1 increases with annealing temperature from RT to 750°C, especially for anatase peaks.
![Page 13: Quang phổ Laser](https://reader035.fdocuments.net/reader035/viewer/2022062222/568159df550346895dc729dd/html5/thumbnails/13.jpg)
PL spectra of titanium oxide films formed at 3, 6, 10 and 15 FO2% and post-annealed at 750 °C for 2 min in air.
RESULTS AND DISCUSSION
The relationship between the crystalline structure and PL behaviors of titanium oxides
Laser excitation: 325 nm, at the room temperature _ The weak shoulder peak at 650 nm is induced from the laser source._ An asymmetrical wide FWHM peak in visible region is observed at the 3 FO2% sample.
![Page 14: Quang phổ Laser](https://reader035.fdocuments.net/reader035/viewer/2022062222/568159df550346895dc729dd/html5/thumbnails/14.jpg)
The Gaussian fitted curve of PL spectra of the 3 FO2% film at 750 °C annealed for 2 min in air.
RESULTS AND DISCUSSION
_ The wide peak is merged from two different TiOx peaks.
_ The curve can be fitted into two Gaussian peaks at 486 nm (2,55eV) and 588 nm(2,11eV).
![Page 15: Quang phổ Laser](https://reader035.fdocuments.net/reader035/viewer/2022062222/568159df550346895dc729dd/html5/thumbnails/15.jpg)
PL spectra of titanium oxide films at 3 FO2% and post-annealed at RT, 350 °C , 550 °C , and 750 °C for 2 min in air.
RESULTS AND DISCUSSION
_ Luminescence shift caused by the mixed anatase and rutile phase. _ The intensity of PL peaks increases with annealing temperature because of enhancement of the crystallinephase._ For the as-deposited and 350 °C annealed samples, the PLsignal is very weak due to the poor crystallinity.
![Page 16: Quang phổ Laser](https://reader035.fdocuments.net/reader035/viewer/2022062222/568159df550346895dc729dd/html5/thumbnails/16.jpg)
The oxygen flow ratios during deposition and post-annealed temperatures result in the evolution of phase formation of the films
CONCLUSION
The XRD and Raman results indicate that the 3 FO2% film is formed of a mixed phase of anatase and rutile, and the specimens of 10 FO2%, and 15 FO2% are the single-phase anatase after 550–750 °C annealing
The as-deposited TiOx films and those annealed at 350 °C are all amorphous because of no distinct diffraction peak.
The minimum thermal annealing temperature necessary to stimulate the crystallization of film is between 350 °C and 550°C.