JPS6326558A - Analysis for ultramicroquantity of uranium - Google Patents
Analysis for ultramicroquantity of uraniumInfo
- Publication number
- JPS6326558A JPS6326558A JP16976986A JP16976986A JPS6326558A JP S6326558 A JPS6326558 A JP S6326558A JP 16976986 A JP16976986 A JP 16976986A JP 16976986 A JP16976986 A JP 16976986A JP S6326558 A JPS6326558 A JP S6326558A
- Authority
- JP
- Japan
- Prior art keywords
- uranium
- wavelength
- pulse laser
- sample
- intensity
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229910052770 Uranium Inorganic materials 0.000 title claims abstract description 22
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 238000004458 analytical method Methods 0.000 title claims description 6
- 238000000034 method Methods 0.000 claims description 4
- 238000012929 ultra trace analysis Methods 0.000 claims description 4
- 238000004611 spectroscopical analysis Methods 0.000 claims description 2
- 230000001678 irradiating effect Effects 0.000 claims 2
- 238000005259 measurement Methods 0.000 abstract description 7
- 239000007787 solid Substances 0.000 abstract description 4
- 238000011088 calibration curve Methods 0.000 abstract description 2
- 230000003252 repetitive effect Effects 0.000 abstract 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 238000001514 detection method Methods 0.000 description 6
- 230000035945 sensitivity Effects 0.000 description 5
- 238000007796 conventional method Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000013256 coordination polymer Substances 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 230000004069 differentiation Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000002795 fluorescence method Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- -1 uranium Chemical compound 0.000 description 1
Landscapes
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
この発明は、ウランの超微量分析法、特にシリカ等の半
導体材料中に含まれるウランの超微量分析法に関するも
のである。DETAILED DESCRIPTION OF THE INVENTION (Industrial Application Field) The present invention relates to a method for ultratrace analysis of uranium, particularly to a method for ultratrace analysis of uranium contained in semiconductor materials such as silica.
半導体の高集積化に伴ない、ソフトエラーの発生原因と
なる放射線発生物質、特にウランの含有量を知ることが
材料管理上重要な問題になってきており、例えば１Ｍバ
イトでのウラン許容量は０．１ＰＰｂ以下の値が要求さ
れ極低ウラン品の開発には高感度分析技術が確立されね
ばならない。As semiconductors become more highly integrated, knowing the content of radiation-generating substances, especially uranium, which causes soft errors, has become an important issue in material management.For example, the permissible amount of uranium in 1MB is A value of 0.1 PPb or less is required, and highly sensitive analysis technology must be established to develop ultra-low uranium products.
（従来技術）
従来のウラン分析法は、第２図に示すようなものであっ
て、Ｘランプ１Ｂからの光を励起側の分光光器１８で分
光した２８０ｎｍの光を励起光源とし、固体試料２０に
照射し、発生した蛍光を蛍光側の分光器２１で分光し４
００〜Ｂｏｏｍｍの範囲で走査した信号を検知器２２で
検出する。光信号は電圧−に変換され、アンプ２３で増
幅されてＡＯ変換器を備えたＣＰυ２Ｂで測定される。(Prior art) The conventional uranium analysis method is as shown in FIG. 20, and the generated fluorescence is separated by a spectrometer 21 on the fluorescence side.
A detector 22 detects a signal scanned in the range from 00 to Boomm. The optical signal is converted into voltage -, amplified by amplifier 23, and measured by CPυ2B equipped with an AO converter.
一方、Ｘランプ１Ｂの変動をモニター検知器２４で検出
し、アンプ２５で増幅した後、ＡＯ変換器を備えたＣＰ
υ２６へ導入する。測定された信号は、Ｘランプ１８の
変動補正や微分などｅ
の信号処理を行った後Ｄ／Ａ変換器２７を介しレコーダ
ー２８に記録する。On the other hand, after the fluctuation of the X lamp 1B is detected by the monitor detector 24 and amplified by the amplifier 25, the CP equipped with an AO converter
Introduced to υ26. The measured signal is subjected to signal processing such as correction of fluctuations in the X lamp 18 and differentiation, and then recorded on a recorder 28 via a D/A converter 27.
これらの操作を試料と標準試料について行い、その比較
によりウランを定量するものである。These operations are performed on samples and standard samples, and uranium is determined by comparing them.
この分析方法においては、試料１ｇを処理して測：ｉ−
：、た場合、測定できる濃度下限的０゜２ｐｐｂ程度一
部って要求される感度及び分析精度を得られな１戸 。In this analytical method, 1 g of sample is processed and measured: i-
: If the measurable concentration is lower than 0.2 ppb, the required sensitivity and analytical accuracy cannot be obtained.
ｒ’ ＩＩ的）
軌発明は、例えば半導体封止材となるシリカフィラー等
のウラン含宥量を志願分解分光分析法によって高感度で
検出定量できる超微量分析法を提供するもので現行分析
法の約５０倍の感度をもって定量できるものである。The invention provides an ultra-trace analysis method that can detect and quantify the uranium content of silica filler, which is used as a semiconductor encapsulating material, with high sensitivity using spontaneous decomposition spectrometry. It can be quantified with approximately 50 times more sensitivity.
（構成）
本発明は、中心波長が２４０＋＋ｍ〜４２０ｎ−のパル
スレーザ−光を２０）１〜１００Ｈの繰り返し周期で固
体ｚ ２
試料に照射し、発生した蛍光又はりん光を分光器によっ
て波＆４００ｒ＋ｍ〜８５０ｎ口の範囲で分光し、この
波長範囲の蛍光又はりん光強度をパルスレーザ−照射後
１ ｇ ｓｅｃ 〜３０ ｇ ｓｅｃ経過後１０ｇ５ｅ
ｃ〜１００ ｈ ｓｅｅの時間幅で測定記録するもので
ある。(Structure) The present invention irradiates a solid Z2 sample with pulsed laser light with a center wavelength of 240++ m to 420 n- at a repetition period of 20) 1 to 100 H, and the generated fluorescence or phosphorescence is detected by a spectrometer as a wave &400 r+m ~. The fluorescence or phosphorescence intensity in this wavelength range was measured at 1 g sec to 30 g sec after pulsed laser irradiation.
Measurements and records are made over a time span of c to 100 h see.
本発明において、パルスレーザ−光源としてはＸｅｃｌ
ガスを用いた中心波長３０８ｎｓのエキシマレーザ−又
は第４高調波２１３８ｎｍノＮｄ：ＹＡＧレーザー或は
窒素レーザー等が好適である。In the present invention, the pulse laser light source is Xecl
An excimer laser using gas with a center wavelength of 308 ns, a Nd:YAG laser with a fourth harmonic of 2138 nm, a nitrogen laser, or the like is suitable.
本発明において、試料からのウランによる蛍光は４００
＋＋■〜８５０ｎｍの波長範囲で観測される。In the present invention, the fluorescence due to uranium from the sample is 400
It is observed in the wavelength range from ++■ to 850 nm.
更にウランの波長５５５ｎ■のスペクトル線についてそ
の蛍光強度が最大の条件を信号検出時点とその測定時間
幅について種々実測したところ信号検出時点つま、り遅
延時間はレーザー照射後１ｕＬｓａｃ〜３０ ｐ、 ｓ
ｅａ特に１２．５１７． ｓｅｃ 〜２５４ ｓｅｃと
するのが最適であることが判った。１ｐ、 ｓｅｃ未満
では散乱光や短時間物質の影響が大きくなりまた３Ｑ
ＪＬ ｓｅｃを超えるとウランの蛍光を感度よく検出で
きない。Furthermore, we actually measured various conditions for the signal detection time and measurement time width under which the fluorescence intensity of uranium's spectral line with a wavelength of 555 nm is maximum, and found that the signal detection time, that is, the delay time after laser irradiation was 1 uLsac ~ 30 p, s.
ea especially 12.517. sec to 254 sec was found to be optimal. If it is less than 1 p, sec, the influence of scattered light and short-time substances becomes large, and 3Q
If JL sec is exceeded, uranium fluorescence cannot be detected with high sensitivity.
また、測定時間幅については１０ｇ５ｅｃ未満では十分
な蛍光強度を得ることができず、１００ ｐ、 ｓｅｃ
を超えると長寿命物質の影響を−受けるので好ましくな
い、好適な時間幅は・１２．５終Ｓｅｃ〜２５終ｓｅｃ
である。In addition, regarding the measurement time width, if it is less than 10 g5 ec, sufficient fluorescence intensity cannot be obtained, and 100 p, sec.
Exceeding this is not preferable because it will be affected by long-lived substances.The preferred time range is 12.5 seconds to 25 seconds.
It is.
上記の時間設定は試料の種類及び処理方法等によって異
なるから実測前に最良の状態が得られるように決定する
のがよい。The above time settings vary depending on the type of sample, processing method, etc., so it is best to determine them before actual measurement so as to obtain the best conditions.
本発明分析方法に適用する装置は第１図のようであって
、（１）はパルスレーザ−１（２）はプリズム、（３）
（４）はミラー、（５）（６）はレンズ、（７）は固体
試料である。The apparatus applied to the analysis method of the present invention is shown in Fig. 1, in which (1) is a pulse laser, (2) is a prism, and (3) is a pulse laser.
(4) is a mirror, (5) and (6) are lenses, and (7) is a solid sample.
分光器（８）で分光された蛍光は、検出手段である光電
子増倍Ｉ′ｒＦ（９）で電気信号に変換される。The fluorescence spectrally separated by the spectrometer (8) is converted into an electrical signal by the photoelectron multiplier I'rF (9), which is a detection means.
（ＩＱ）（１７）は電源、 、（１１）はアッテネータ
−１（１２）はアンプ、 （１３）はボックスカー積分
器、（１４）はシンクロスコープ、（１５）はレコーダ
である。パルス発生器（１Ｂ）は、パルス幅 １ｍ５ｅ
ｃの短形波を発生する。このタイミングパルスはパルス
レーザ−の照射時点に同期して発生され、その繰り返し
周期は２０Ｈ２〜 １００Ｈ２に設定されボー７クス力
−積分器（１３）シンクロスコープ（１４）等に入力さ
れ夫々の動作時点を制御している。(IQ) (17) is a power supply, (11) is an attenuator, (12) is an amplifier, (13) is a boxcar integrator, (14) is a synchroscope, and (15) is a recorder. The pulse generator (1B) has a pulse width of 1m5e.
Generates a rectangular wave of c. This timing pulse is generated in synchronization with the irradiation point of the pulsed laser, and its repetition period is set to 20H2 to 100H2, and is input to the Vaux force integrator (13), synchroscope (14), etc. at each operating point. is under control.
（実施例）
（１）試料シリカＩｇを白金皿に入れ硝酸とツー２酸を
加えてホットプレート上で分解管乾固させた。(Example) (1) A sample of silica Ig was placed in a platinum dish, nitric acid and dioxylic acid were added, and the decomposition tube was dried on a hot plate.
これにＮａＦ 、 Ｈａ、、Ｇｏ３． Ｋ２ｆ、０３混
合の融剤を加え融解冷却固化させ、直径３０ｍｍφ程度
の固体試料を作成した。To this, NaF, Ha, Go3. A mixed flux of K2f and 03 was added, melted, cooled, and solidified to prepare a solid sample with a diameter of about 30 mmφ.
（２）レーザーを発振させサイラトロンへの供給電圧の
周期を設定し、レーザー発振の繰り返しを２０Ｈｚ〜
１００）！２の範囲で決定する。(2) Set the cycle of the voltage supplied to the thyratron by oscillating the laser, and repeat the laser oscillation at 20Hz~
100)! Decide within the range of 2.
（３）プリズム、ミラー、レンズの調整により光軸の調
整を行なう、この場合、レーザー光が試料に１０〜２０
ｍｍφの大きさで均一に照射される様に調整する。また
、試料からの蛍光が分光器スリットの中心へ集光する様
に調整する。(3) Adjust the optical axis by adjusting the prism, mirror, and lens.
Adjust so that it is irradiated uniformly with a size of mmφ. Also, adjust so that the fluorescence from the sample is focused on the center of the spectrometer slit.
（４）分光器（８）の波長を最も強い信号が得られる波
長５５５ｎｍに合せ、ボックスカー積分窓、シンクロス
コープ、レコーダーの各レンチ及ヒアンプの増ｌ１１ｉ
率をレコーダーの範囲内に信号が納まる様に設定する。(4) Adjust the wavelength of the spectrometer (8) to the wavelength 555 nm that gives the strongest signal, and increase the boxcar integration window, synchroscope, and recorder wrench and amplifier l11i.
Set the rate so that the signal falls within the range of the recorder.
（５）シンクロスコープにより、減衰曲線をモニターし
、信号検出の開始時間及び信号検出の時間範囲を設定す
る０本例の場合は、信号検出の開始時間はレーザー光を
試料に照射後２０ ＩＬｓｅｃまた測定時間範囲は２５
ＪＬ ｓｅｃとした。また、ボックスカー積分器への
入力信号の調整は、検出器であり光電子増倍管への印加
電圧及び分光器のスリット幅により調整する。(5) Monitor the attenuation curve using a synchroscope and set the signal detection start time and signal detection time range. In this example, the signal detection start time is 20 ILsec or The measurement time range is 25
JL sec. Further, the input signal to the boxcar integrator is adjusted by the voltage applied to the photomultiplier tube, which is a detector, and the slit width of the spectrometer.
（６）分光器の波長を４００ｎ腸に設定し、分光器の波
長とレコーダーとを同期させて駆動する０分光波長（７
）Ｒ囲は４００＋ｍ〜８５０ｎｓとし、レコーダーに記
録する。(6) Set the wavelength of the spectrometer to 400 nm, and synchronize the wavelength of the spectrometer and the recorder to drive the 0 spectral wavelength (7
) R radius is set to 400+m to 850ns and recorded on a recorder.
（７）最大強度を示すピークのピーク強度又はピーク面
積を算出し、あらかじめ作成しておいた検量線又は、濃
度既知の標準試料との比較により含有ウラン量を計算す
る。(7) Calculate the peak intensity or peak area of the peak showing the maximum intensity, and calculate the amount of uranium contained by comparing it with a calibration curve prepared in advance or a standard sample of known concentration.
第３図Ａ、Ｈに従来法により測定したウランＩ ＰＩ）
ｋｌと ５ ＰＰｂのスペクトルを示し、第３図Ｃに水
沫より測定したウラン０．Ｉ ＰＰｂのスペクトルを示
す゛、この結果より水沫は従来法に較べ少なくとも５０
倍は感度が良いことがわかる。Figure 3 A and H show uranium I (PI) measured using the conventional method.
The spectra of kl and 5PPb are shown, and Figure 3C shows the uranium 0.0% measured from water droplets. The spectrum of IPPb is shown. From this result, the water droplet is at least 50% lower than that of the conventional method.
It can be seen that the sensitivity is twice as good.
（発明の効果）
本発明によれば、試料調整時の処理に関係なく蛍光測定
の際に不純物の影響を除くことができ、かつ装置に特別
の装置又は器具を必要とすることなく ０．０１ ｐｐ
ｂ程度の極微量ウランでも高精度に定量することができ
るのである。(Effects of the Invention) According to the present invention, the influence of impurities can be removed during fluorescence measurement regardless of the processing during sample preparation, and 0.01 without requiring any special equipment or instruments in the apparatus. pp
Even extremely small amounts of uranium, such as uranium, can be quantified with high precision.
第１図は本発明装置の構成図、第２図は従来の固体蛍光
法による装置の構成図である。第３図は従来法（Ａ、Ｂ
）と水沫（Ｃ）により蛍光強度を波長の関数として測定
したスペクトルの比較図。
第４図は、蛍光波長５５５＋ｍにおける蛍光強度を時間
の関数として測定した減衰曲線を示したものである。
（１）・・・パルスレーザ−
（７）・・・試料
（８）・・・波長駆動装置付き分光器
（９）・・・ホトマルチ
（１３）・・・ボックスカー積分器
（１４）・・・シンクロスコープ
（１５）・・・レコーダーFIG. 1 is a block diagram of an apparatus according to the present invention, and FIG. 2 is a block diagram of a conventional apparatus using a solid-state fluorescence method. Figure 3 shows the conventional method (A, B
) and water droplets (C). Comparison of spectra of fluorescence intensity measured as a function of wavelength. FIG. 4 shows a decay curve of the fluorescence intensity measured as a function of time at a fluorescence wavelength of 555+m. (1)...Pulsed laser (7)...Sample (8)...Spectrometer with wavelength drive device (9)...Photomulti (13)...Boxcar integrator (14)...・Synchroscope (15)...Recorder
Claims (2)
って発生した蛍光又はりん光の強度を時間及び波長の関
数として測定するウランの時間分解分光分析法において
、波長が紫外域であるパルスレーザー光を試料に照射し
て得られる波長４００ｎｍ〜６５０ｎｍの範囲の特定波
長光を前記レーザーパルス照射後１μｓ〜３０μｓの時
間内において１０μｓ〜１００μｓの時間巾で検出して
ウラン濃度を測定することを特徴とするウランの超微量
分析法。(1) In time-resolved spectroscopy of uranium, which measures the intensity of fluorescence or phosphorescence generated by irradiating a fixed sample with pulsed laser light as a function of time and wavelength, pulsed laser light with a wavelength in the ultraviolet region is used. The uranium concentration is measured by detecting light with a specific wavelength in the range of 400 nm to 650 nm obtained by irradiating the sample with a time width of 10 μs to 100 μs within 1 μs to 30 μs after the laser pulse irradiation. Ultratrace analysis method for uranium.
ある特許請求の範囲第１項の分析法。(2) The analysis method according to claim 1, wherein the center wavelength of the irradiated laser beam is 240 to 420 nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16976986A JPS6326558A (en) | 1986-07-21 | 1986-07-21 | Analysis for ultramicroquantity of uranium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16976986A JPS6326558A (en) | 1986-07-21 | 1986-07-21 | Analysis for ultramicroquantity of uranium |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS6326558A true JPS6326558A (en) | 1988-02-04 |
Family
ID=15892514
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP16976986A Pending JPS6326558A (en) | 1986-07-21 | 1986-07-21 | Analysis for ultramicroquantity of uranium |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6326558A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006005905A3 (en) * | 2004-07-08 | 2006-04-27 | British Nuclear Fuels Plc | Method for the handling and minimisation of waste |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60211339A (en) * | 1984-03-16 | 1985-10-23 | コミサリヤ・ア・レネルジ・アトミク | Method of determining trace of uranium in solution |
-
1986
- 1986-07-21 JP JP16976986A patent/JPS6326558A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60211339A (en) * | 1984-03-16 | 1985-10-23 | コミサリヤ・ア・レネルジ・アトミク | Method of determining trace of uranium in solution |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006005905A3 (en) * | 2004-07-08 | 2006-04-27 | British Nuclear Fuels Plc | Method for the handling and minimisation of waste |
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