Basic Service-Material-X-ray Photoelectron and Auger Electron Epectroscopy-NYCU Office of Research and Development

Basic Service-Material

中文

Update Date：2024-02-06
Units：Instrumentation Resource Center

X-ray Photoelectron and Auger Electron Epectroscopy

X-RAY PHOTOELECTRON & AUGER ELECTRON SPECTROSCOPY

X-ray Photoelectron and Auger Electron Epectroscopy
English abbreviation: XPS/AES
Brand model: UK Thermo Fisher Scientific, ESCALAB Xi⁺
Instrument expert: Prof. Hsu, Yung-Jung
ext 55317
Email yhsu@cc.nctu.edu.tw
Instrument consultation and operation service: Ms. Huang, Hsiu-Ying
Extension 55358 (EF110 Office), 55339 (EF215 Laboratory)
Email yuffie@nycu.edu.tw
Instrument location: Room EF215, Engineering Building 6, Guanfu Campus
ext 55339

Instrumentation

Chinese name: X-ray photoelectronics and Oujie electronic energy spectrometer
English name: X-ray Photoelectron and Auger Electron Epectroscopy
Year and month of joining Guiyi: November 2004
Year and month of instrument purchase: November 2017, replacing old ones with new ones
Instrument funding sources: National Science Council, National Yang-Ming Chiao Tung University
Brand and model: British Thermo Fisher Scientific, ESCALAB Xi+

Important Specifications

XPS (ESCA):
- X-ray light source: monochromatic X-ray source (Al Anode)
- The X-ray beam can be set from 200μm to 900μm
Energy analysis instrument: 180° Spherical Sector Analyzer (SSA)
- Energy resolution: 0.02~2.0%
- Energy resolution≦ 0.5eV at Ag 3d5/2 peak (Ag standard)
- Energy resolution≦ 0.9eV at C 1s peak (PET standard)
- Analysis area: 20μm~8mm
Ion source: Argon ion gun
- Two sputtering modes, Monatomic and Cluster, are available for sample surface cleaning and in-depth analysis.
- Ion beam energy range:
  - Monatomic mode─500 eV to 3 keV
  - Cluster mode─2 keV to 7 keV
- Ion beam size range:
  - Monatomic mode─500 μm @ 3.0 μA and 3 keV
  - Cluster mode─100 atoms ~ 2000 atoms
Single-gun dual-beam charge compensation: The same beam source can simultaneously use low-energy electrons and ions for dual-beam charge compensation.
AES: field emission electron gun
- Acceleration voltage: 1 keV ~ 10 keV
- SEM spatial resolution: 95 nm at 10 keV, 5.0 nA
UPS (Ultraviolet Photoelectron Spectroscopy):
- Ultra Violet source (He UV light source)
- Test piece size: 5mm×5mm ~40mm×20mm
- Vacuum rate: ~30 minutes

Function

XPS qualitative and quantitative analysis of surface components
XPS chemical shift analysis
XPS depth profile analysis
XPS element image scanningXPS Mapping
UPS UV photoelectron scanning
Auger surface composition analysis
Auger depth profiling depth component analysis
Auger point analysis and mapping micro-area element and component distribution analysis
REELS/ISS
Electrical neutralization charge compensation

1. Service items and content
	Service items	Possible information content
1	Qualitative surface analysis (Survey Scan)	Identify the presence of various chemical elements on the surface of the sample
2	Surface Quantitative Analysis (Survey Scan)	Identification of the relative atomic concentration percentage of elements on the surface of the sample
3	XPS chemical shift (chemical shift)	Analyze the chemical state/bonding state of elements
4	Depth profiling	The depth distribution of various chemical elements in the sample under ion etching
5	Micro area analysis (Point)	Identification of the components of selected micro-areas on the surface of the sample
6	Element image scanning (Mapping)	Obtain the two-dimensional distribution image of chemical elements on the sample surface
7	Ultraviolet photoelectronic scanning (UPS)	Measurement of Valance band and work function
8	REELS(Reflection Electron Energy Loss Spectroscopy)	Identification of allotropes

2. Open usage time and management
	8:30~12:30am	13:30～17:30 pm	18:00～22:00 in the evening
Monday	Instrument Maintenance	Entrusted service period (priority registration outside campus)	Self-operated period (Level B) (priority registration on campus)
Tuesday	Self-operated period (Level B) (priority registration outside school)	Entrusted service period (priority registration on campus)	Self-operated period (Level B) (priority registration on campus)
Wednesday	Entrusted service period (priority registration on campus)	Entrusted service period (priority registration outside campus)	Self-operated period (Level B) (priority registration on campus)
Thursday	Training period	Entrusted service period (priority registration on campus)	Self-operated period (Level B) (priority registration on campus)
Friday	Assessment period	Entrusted service period (priority registration outside campus)	Self-operated period (Level B) (priority registration on campus)
Saturday	Self-operated period (Level A)	Self-operated period (Level A)	Self-operation period (level A)
Sunday	Self-operated period (Level A)	Self-operated period (Level A)	Self-operation period (level A)

Level B: Open to students who need to use it. They can operate it on their own after training and assessment.
Level A: Only those with Level B licenses who have accumulated 80 hours of computer time can apply for the exam to become Level A licenses.

Application Service Methods (Reservation rules are subject to the National Science Council Basic Research Core Facilities Reservation Service Management System, and the time period is flexible)

Technician Operation Service:
1. Please go to National Science Council Basic Research Core Facilities Reservation Service Management System Reservation period (Reservations for the next month will be open at 00:00 am on the 21st of each month, Make a priority appointment according to the table above; for off-campus priority time slots, if the reservation is not full after 7 days of opening, the technician may open the appointment to people inside and outside the school). Detailed description of the nature of the sample to be tested and the entrusted items will be provided according to the time period applied for. For those who want to make an appointment, please refer to Relevant regulations to avoid incorrect payment methods. If for some reason the film to be tested cannot be delivered before the appointment time, you should cancel the appointment online at least one week before the appointment time. If you do not arrive for the appointment, you will still be charged for the original appointment time period.
2. Each entrusted user can only reserve 7 time periods/month (four hours is a time period), the number of samples sent for each test: Depth: 1 sample/time period , Surface analysis: The maximum number of elements to be analyzed is 30 in total per period. Reservations can be made only after the measurement is completed; those who do not meet the requirements will be automatically canceled without further notice.
3. When capturing micro-area positioning maps or images, someone must accompany the unit sending the test.
4. Interpretation of data results is your own responsibility.
5. If the sample is submitted for testing without prior written request for sample pre-processing and the desired spectrum cannot be obtained, the unit submitting the sample still needs to pay according to the working hours.
6. Please bring a blank CD-ROM, pen drive or blank diskette for analysis data access.
7. A valuable instrument reservation application form must be submitted (the supervisor’s signature is required).
Self-operated services:
1. Doctoral students who have obtained "qualified licenses" can operate the computer on their own.
2. Reservations for the use of self-operated instruments are based on the laboratory. The number of reservations is limited: 5 periods/month. Reservations can be made only after the measurement is completed. Those who do not meet the regulations Will be automatically canceled without notice.
3. Self-operators must call the technician to make an appointment before each use. You can make another appointment after the test is completed.
4. If for some reason you are unable to use the instrument during the reservation period, you should cancel the reservation online at least one week before the reservation period, otherwise you will still be charged for the original reservation period.
5. When the sample enters, the pressure of the entry chamber of the instrument system must reach 1×10-3torr.
6. Before sample analysis, the analysis chamber pressure of the instrument system should be determined<5×10-9torr before turning on the electron gun and detector power switch for analysis.
7. When using this instrument, any damage caused by abnormal use will be borne by the operator's instructor and supervisor to bear the maintenance costs of the instrument and equipment.
8. Instrument users must fill in the experiment record book accurately.
9. It is prohibited to bring food and drinks into the instrument room for consumption, and the instrument room must be kept clean and tidy.
10. Must comply with the X-ray Optoelectronics and Oujie Electronic Energy Spectrometer Laboratory Management Regulations.
Sample specifications:
1. Samples must not be liquid, powder, toxic, magnetic, radioactive, organic (including film) or cause corrosion to vacuum chamber parts.
2. Samples should be limited to low non-volatility to avoid contamination of the ultra-high vacuum system.
3. The area is larger than 0.5cm * 0.5cm square, smaller than 4cm *2cm rectangle, and the thickness is < 2mm.
4. Please send two samples for the testing service in case of testing difficulties.
5. If during analysis and testing, it is found that the sample submitted for testing does not meet the requirements, the sample will be returned and payment will be made based on the working hours.
6. When performing depth profile, the sputter time is limited to 3.5 hours. Please consider the thickness of the test piece by yourself.
How to obtain a qualified license

Purpose: In order to make full use of this valuable instrument, we decided to open it to qualified users. , to relieve excessive service demands and reap the benefits of talent training.

Method: How to obtain a "Use License":

Each research office should recommend a doctoral student by the supervising professor or unit supervisor to submit an application.
Application qualifications: Applicants must have studied relevant material analysis technology courses and have experience in operating electron microscopes.
The doctoral student should fill out the "Education and Training Application Form" (Level A or B) and arrange training time through the instrument technician.
This instrument will provide educational training and use "training operation" and "operation observation" methods to achieve the purpose of self-operation in the laboratory of the main user. "Training operation": the teaching assistant is responsible for teaching the machine structure and operation steps; "Operation observation": learning the operation skills from qualified licensed users.
The number of B-level training is 4 weeks, and operation observation requires more than 2 times; the number of A-level training is 2 weeks.
Those who pass the operation examination by the teaching assistant or technician and the professor in charge of the instrument will obtain the qualification of "Qualified Level B or Level A Operator".
Level B operators must accumulate more than 80 hours of operation before they can apply for the qualification of Level A operators.
After the doctoral student obtains the [User License], he needs to assist his own laboratory personnel in performing the analysis of this instrument.
If additional practice operations are required (a qualified operator must be present), the fees will be charged according to technician operation services (charge standard: 450 yuan per hour).
If you fail the operation test for the second time and make serious mistakes during operation, the laboratory reserves the right to refuse the trainee the right to operate it in person.
When using this instrument, any damage caused by abnormal use will be borne by the instructor and supervisor of the self-operated instrument and equipment maintenance costs.
If a user who has obtained a "qualified license" does not operate this equipment for 2 months, his or her qualifications will need to be re-certified.
Must comply with laboratory regulations during training and use.

Charging standards

Entrusted service:
The charging standard is a basic usage fee of NT$500/hr, which is billed based on the time period. If the service exceeds 4 hours, the actual service hours will be billed. Including sample processing time, sample vacuuming time, shutdown waiting time and data processing time, late time will still be billed as service time.
- Use Ar ion gun NT$100/hr.
- Use charge compensation gun NT$100/hr.
- Use UPS NT$120/hr.
- Emergency charges are twice the standard charges.
Self-operation: The charging standard is the basic usage fee of NT$400/hr, and the rest are the same as entrustment.
The fees for education and training are all billed according to technician operation services (charge standard: NT$500 per hour). For B-level training, please reserve four sessions; for A-level training, please reserve one session. And explain the reservation used for training.