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高解析度小角度X光散射儀 (SAXS)

儀器名稱:高解析度小角度X光散射儀((Small Angle X-Ray Scattering System, SAXS)

l購置年度:94年

l放置地點:第二教學大樓(T2-102)

l服務項目:

一、一般測量(General Measurements(固態樣品、室溫、抽真空、及穿透模式下測量))

1. 小角度X光散射測量(Small Angle X-ray Scattering, SAXS)

散射角2q為0.07-2.2o, 散射向量k (=4psinq/l, nm-1) range為5.4 x 10-2 - 1.6, D-spacing為115-3.8 nm。

2. 中角度X光散射測量(Medium Angle X-ray Scattering, MAXS)

散射角2q為0.22-6.7o, 散射向量k (=4psinq/l, nm-1) range為0.16 - 4.8, D-spacing為38-1.2 nm。

3. 廣角度X光散射測量 (Wide Angle X-ray Scattering, WAXS)

散射角2q為6.5-67o, 散射向量k (=4psinq/l, nm-1) range為4.6 - 45, D-spacing為1.3-0.14 nm。

但如有特別需求,散射角2q的測量範圍可調為2 - 67o (此時,吾人可使用中心鑽有直徑為3.2 mm小洞的image plate;一般的image plate,其中心鑽的小洞直徑為7 mm,故最低的散射角只能測至約6.5o)

二、20-300C變溫測量(SAXS Measurements at varied temperatures from 20 to 300 C)(固態樣品、抽真空、及穿透模式下SAXS測量)

三、液態樣品測量(Measurements for liquid sample) (液態樣品、室溫或變溫、抽真空、及穿透模式下測量)

四、固態樣品低掠角/反射度測量(Measurements for solid sample using grazing incidence/reflectivity module, SAXS)

已於2013/5/1正式開放對外服務

五、常壓下測量(Measurements under ambient pressure, SAXS或WAXS)

l樣本準備需知

一、室溫測量條件下,固體樣品試片或薄膜尺寸 (size suggested for solid specimen or film under room temperature):3 to 5 cm (length), 0.5 to 1 cm (width), and less than 1 to 2 mm (thickness). (The sample will be fixed on a sample rack with 42 holes (about 1 cm in diameter) on it using a 3M Scotch tape.)

二、變溫測量條件下(20-300C),固體樣品試片或薄膜尺寸 (size suggested for solid specimen or film under varied temperature (20-300 C)):0.5 cm (length), 0.5 cm (width), and less than 1 to 2 mm (thickness). (The sample will be placed on a temperature-controlled liquid sample cell with sample size limitation mentioned above.)

三、固體粉末數量 (amount of powder): at least 0.5 to 1 cubic cm of the powder should be provided. (The sample will be put into a special quartz capillary (1 or 2 mm in OD, 0.1 mm in wall thickness, and 80 mm in length, which is imported from USA), and its one end will be sealed with a tape.)

四、固態樣品需無毒、無(或極低)揮發性、且無輻射性 (The sample should be free from poison, volatility, and radiation.)

室溫測量條件下(20℃),低黏度液體樣品溶液: at least 0.5 to 1 cubic cm of the low-viscosity liquid sample should be provided. (The sample will be put into a special quartz capillary (1 or 2 mm in OD, 0.1 mm in wall thickness, and 80 mm in length, which is imported from USA), and its one end will be sealed with epoxy.) Please be noted that the user should also provide at least 0.5 to 1 cubic cm of pure solvent sample for the X-ray scattering experiment in order to facilitate the background subtraction from the sample solution.

五、樣品若需沈積在基板上,基板的材質及厚度,不可讓X-ray對基板的吸收度高於90%以上,否則樣品將無法在穿透模式下測量。建議使用0.1mm厚度以下的矽晶片或石英玻璃片為佳。(If the sample has to be deposited on a substrate, the material and thickness of the substrate should not cause the degree of absorption of the incident X-ray greater than 90%. Otherwise, the sample will probably not be able to be measured its scattered intensity under the transmission mode of the test. It is suggested to use silicon wafer or quartz glass plate with a thickness less than 0.1 mm.)

l 收費標準:

計費項目 計費單位 計費數量 計費單價
儀器使用費(科技部計畫 小時 4 32000
儀器使用費(全額現金 小時 4 6000
盛裝粉末樣品用石英毛細管耗材(科技部計畫) 1 4000
盛裝粉末樣品用石英毛細管耗材(現金付費) 1 400

1. 自民國98年4月1日起,計畫付費的使用者,每服務單元(4小時)之收費標準調高為新台幣32000元;自2005/6/6起,使用本實驗室準備自美國進口之石英毛細管者,每枝毛細管額外收取新台幣4000元(四仟元)材料費。

2. 現金付費的使用者,每服務單元(4小時)之收費標準為新台幣6000元;使用本實驗室準備自美國進口之石英毛細管者,每枝毛細管額外收取新台幣400元(四佰元)材料費。

*  使用本實驗室準備自美國進口之石英毛細管者,每枝毛細管額外收取新台幣400元材料費(限現金,請至本校總務處出納組繳納)。

** 一個服務單元為4小時;未滿4小時,一律以4 小時計。

***實驗結果及圖形,在您的服務單元結束後,立即取回。請自備隨身碟儲存檔案資料。

l開放服務對象:校內、校外學術單位及產業界

Service Time for High Resolution SAXS System

Mon Tue We Thur Fri
8:30 am-12:30 noon 3 2 1 2 1
13:30 pm-17:30 pm 3 2 1 2 1

1: 校內貴儀使用者預約 (reserved for faculty members or graduate student at NTUST having MOST account entitled to use precious instruments of the MOST-sponsored labs)

2: 校外貴儀使用者預約 (reserved for faculty members or graduate student from other university or research organization having MOST account entitled to use precious instruments of the MOST-sponsored labs)

3: 願意繳交現金之使用者預約 (reserved for applicants willing to pay cash to use the SAXS system)

4: 每月第二及第四個週一,儀器停機一天,更換針孔系統及光束停止點。遇假日則順延至次一個上班日。 (For the second and fourth Monday of each month, the SAXS system will be down for changing the pinhole and beamstop. Should it be a holiday for that Monday, the down time for the SAXS system will be delayed to the nearest working day.)

l儀器負責老師及技術員聯絡方式:

儀器負責老師:黃延吉教授

TEL:(02)2737-6625

E-mail:huangyj@mail.ntust.edu.tw

技術員:張美杏小姐

TEL:(02)2730-1028

E-mail:maigge@mail.ntust.edu.tw

l儀器介紹:

一、說明

小角度X光繞射儀(SAXS)是用來研究大小尺寸在1 nm (奈米)至100 nm之材料結構1-2。該項結構資訊通常係藉由測量X光散射強度I(q)對散射向量q的變化得之,其中q = 4psinq/l,此處l為入射X光波波長,2q為散射角。根據Bragg定律sinq=l/2d, 當代表材料結構中之重覆週期、結晶面之間距、或規則結構之微相區的距離d為1 nm至100 nm大小時,若l以0.154 nm計算(CuKa光源),則散射角2q約為9o 至0.09o

SAXS儀器主要可用來從事「高分子物理」的研究, 可研究的範疇包括:

(ⅰ) 稀薄粉粒体(particulate)系統中的高分子形狀及大小的測定。

(ⅱ) 非粉粒体兩相系統中的相溶性、平均相區大小、兩相界面面積及兩相界面厚度。

(ⅲ) 相溶之高分子聚摻系統中的熱力學相分離行為。

(ⅳ) 週期系統中的材料結構分析,如結晶性高分子具片狀晶區的堆排者或團聯共聚合物具規則且相分離之微相區者。

(ⅴ) 多層高分子薄膜的反射率(reflectivity)。

(ⅵ) 非均勻高分子材料的分析,如高分子複合材料中的空氣孔隙大小分佈及体積分率的測量。

(ⅶ) 插入型(intercalate)及脫層型(exfoliate)高分子奈米複合材料的鑑定。

二、儀器特色簡述

1. 廠牌與型號: Osmic, USA; PSAXS-USH-WAXS-002

      2. X光源特點: 30 Watts low power x-ray source/optic combination that provides Cu K alpha radiation with comparable intensity to a focused        beam from a rotating anode generator; X-ray source operating at 45 KV, and 0.67 mA. (Model for X-ray

      3. 光束大小: 30 micrometer x 30 micrometer

4. 測量特色:可同時測量小角散射及廣角散射

三、本儀器主要可分為三大部分,其規格特色如下:

(1) Source(光源)

a. Microsource with confocal beam conditioning optic(具點收束型集光鏡之微X光源)

i. Provides monochromatic beam with intensity greater than focused radiation from existing rotating anodes with the exception of the Rigaku 007.(提供單一波長之光束,其光束強度高於,除了Rigaku007以外,現有之旋轉陽極靶所產生之聚焦輻射。)

ii. Operates at only 35 Watts and uses 110V VAC; no special power requirements needed(在35瓦的低功率下操作,並使用110伏特的交流電壓;不需特殊的功率。)

iii. Maintenance comparable to a conventional sealed tube source. (維修與傳統的密封管式的X光光源一樣簡單)

(2) Camera(相機):

a. 3 pinhole geometry with user-exchangeable pinholes(具使用者可更換針孔之三針孔幾何系統)

i. Pinholes can be exchanged for variable flux/resolution without dismantling the entire system. (針孔可更換,以調整光束通率及解析度,不需拆除整個系統。)

ii. Pinholes can be moved out of the way to expose a large through-hole for sequential pinhole alignment. (針孔可移開自原有光徑,以便暴露一個大的貫通孔洞,以利連續之針孔對齊調整)

b. Open Platform design. (開放式平台設計)

i. The only system to offer additional scattering chambers (for different k-space ranges), simultaneous wide angle scattering using image plates, and a surface scattering/reflectivity stage, to name just a few unique options. (本系統獨一無二,提供了額外的散射室(以適用於不同的散射向量空間之範圍),可同時以影像板測量廣角度散射,及提供測量表面散射/反射度的工作台,以上僅略舉數例。)

c. Large sample chamber with the optional ability to cover the incident and scattered beam paths with windows for samples in ambient or other non-vacuum environment.( 大型的樣品室,具含蓋入射及散射光束路徑的選擇能力,並開有視窗,以利常壓或非真空環境下的樣品測量。)

d. The sample changer drive mechanism is mounted outside the sample chamber to maximize the available space inside the chamber.( 樣品更換器驅動機制是安裝於樣品室之外,以使樣品室內的可用空間最大化。)

e. An x-ray photodiode is provided inside the sample chamber to be used for performance diagnostics and also fine tuning the alignment of the monochromator optic and the pinhole positions. (提供一個X射線光電二極管於樣品室內,用以診斷操作性能,及微調單光器光學系統是否對齊及針孔位置。)

f. Video display of the beam position on the sample simplifies the alignment of small samples. (打在樣品上的光束位置,可於影像上顯示,這簡化了小樣品的對齊調整過程。)

g. The beamstop is embedded with an x-ray sensitive photodiode for in-situ transmission measurement. (光束停止點嵌入了一個對X射線敏感之光電二極体,以提供穿透X光強度的即時測量功能。)

(3) Detector(偵測器) :

a. 2D Multiwire, gas-filled proportional type with(二維、多接線、充氣比例類型具有):

i. 120mm active diameter(120毫米之有效直徑。)

ii. Sub-microsecond time stamping for performing time resolved or periodic pump/probe experiments without waiting for data storage. (次微秒時間印記功能,以執行時間分離或週期性之泵送/探測實驗,不需等待資料儲存。)

本儀器的詳細規格,可參閱網頁:http://web.ntust.edu.tw/~HUANGYJ/saxs.htm

 

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