CN85107621A - Pehanorm (TAM) crystal and growth method and the application in x-ray spectrometer - Google Patents
Pehanorm (TAM) crystal and growth method and the application in x-ray spectrometer Download PDFInfo
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- CN85107621A CN85107621A CN85107621.1A CN85107621A CN85107621A CN 85107621 A CN85107621 A CN 85107621A CN 85107621 A CN85107621 A CN 85107621A CN 85107621 A CN85107621 A CN 85107621A
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Abstract
A kind ofly be suitable for crystalline material and the growth method thereof that X-ray spectral analysis is used, this crystal is grown with aqueous solution cooling method, and solvent for use is a water, seed crystal be shaped as strip, the growth temperature interval is 60 ℃---room temperature.This crystal can be with the cutting of the yarn that gets wet, goes out the wafer of desired size with the blade cleavage, makes optical flat or bent crystal X ray monochromator.This crystalline (020) face, 2d value are that 8.78 are strong diffraction surfaces, have the diffraction property that is better than PET crystal (002) face, the sensitivity for analysis height, and the long speed of crystal is fast, and growth cycle is short, the yield rate height, good mechanical property can replace PET to be used for making monochromator on the X-ray spectral analysis instrument.
Description
The present invention relates to be used for the crystalline material and the growth method thereof of X-ray spectral analysis.
Analyzing crystal is the heart element of x-ray spectrometer, it is widely used in electronic probe spectrograph and XRF spectrometer, also is used for sun surface X ray spectral distribution and the measurement of laser fusion plasma electron temperature and the analysis of solid electronic band structure etc.
The analyzing crystal that x-ray spectrometer must dispose several different crystal face distances makes the topped whole X ray spectrum of diffraction wavelength.
The analyzing crystal that Eugene P.Bertin in 1969 report is used for x-ray spectrometer has kind more than 70, and analyzing crystal commonly used has only the LiF(lithium fluoride), quartzy, EDdT(ethylenediamine tartrate), the PET(tetramethylolmethane), the KAP(Potassium Hydrogen Phthalate), the LSD(lead stearate) etc.EDdT(020) 2d=8.80
, be usually used in the Ka characteristic X-ray analysis of elements such as Si, P, S, Cl, Ti, Cr, Mn, Fe, seeking and manufacture experimently new crystal is one of important channel of improving X-ray spectral analysis sensitivity, tolerance range and resolving power.
F, L, Chan nineteen sixty-eight (" Analytical Chemistry " Vol, 40, NO.5 346-369) have reported laboratory growth tetramethylolmethane PET crystalline message, its diffraction efficiency is 2.5 times of EDdT, is 9 times of (to SiKa) .PET(002 of micaceous) 2d=8.75
, the PET crystal is with the static growth of aqueous solution cooling method.We developed the PET crystal since 1969, reported the PET crystalline and grow in 1978.
PET is a medium-long wave band analyzing crystal commonly used at present, and its main drawback is that the high order diffraction inhibition is poor, and the crystal thermal expansivity is big, and crystal is more crisp, ruptures easily when making bent crystal device and standing the big temperature difference.Particularly the growth difficulty of large-size crystals is bigger, and the speed of growth is slow, and the cycle is long, and yield rate is low.
The invention reside in exploration and develop a kind of new x-ray spectrophotometry crystal, make its growth fraction PET easy, and performance is better than PET, can replace PET and obtain better result of use in X-ray spectral analysis.
Pehanorm chemical formula (CH
2OH)
3CNH
2, be called for short TAM.Nineteen fifty-five Rose, H, nineteen eighty-two Engin Kendi report respectively and obtain the small-crystalline used for crystal structure analysis from 20% water and Virahol and methyl alcohol, do not see the document and the patent that the TAM large single crystal growth are arranged and be used for x-ray spectrophotometry crystal.We have measured TAM crystalline complete structure with four garden diffractometers: belong to rhombic system, a=7.786(2), b=8.785(1), C=8.835(1)
, spacer P2
1Cn(C
2V 9), structure cell molecule number Z=4, R=0.049, R
W=0.057, D
V=1.331gcm
-3, M=121.14, mp=168～172 ℃.
The growth of TAM crystal by adopting aqueous solution cooling method.We have measured solubleness one temperature curve of TAM, and the expression of solubleness is St=11.0+2.18t.Water is a solvent, prepares 40～60 ℃ saturated solution.This saturated solution is alkali.Choose the complete small-crystalline of profile and do seed crystal, seed crystal is introduced, drive sincere crystalline style with reversible motor and rotate 30 rev/mins of rotating speeds with sincere crystalline style.Control suitable rate of temperature fall, the cooling amount increases gradually with crystal growth, avoids the temperature fluctuation in the process of growth, can obtain transparent complete large size single crystal, the interval 60 ℃-room temperature of crystalline growth temperature.
By using dimensional requirement, the yarn cutting with band water polishes on silk with described TAM crystal, is cleaved into the wafer of desired thickness with thin blade along (020), is contained on the mask pattern of instrument and has just made crystal monochromator.
The intrinsic parameters that we have tested TAM crystal (020) and PET crystal (002) with double-crystal diffractometer, P(diffraction peak coefficient), W(peak half width R(integrated reflection coefficient)).The result of contrast test shows that the P value of TAM is more bigger than PET, and the R value is littler than PET, and the W value is than little many of PET, and the P/R value is bigger several times than PET.Illustrate that the TAM crystal is better than PET to the diffraction property of X ray, has better resolving power and sensitivity.The experiment of high order diffraction shows TAM(020) than PET(002) good many of the rejection of high order diffraction.The TAM crystal is applied to produce daily on JXA-3A and the metallurgical institute of daily output JCXA-733 electronic probe and the Shanghai Xray fluorescence spectrometer to Cr, Mn, Fe, Cl, Si sample analysis, do the contrast test with PET, prove that also TAM is better than PET to the X-ray spectral analysis effect.
The TAM crystal is a kind of new x-ray spectrophotometry crystal, TAM(020) 2d=8.78
With PET(002) close, the scope of ultimate analysis is identical with PET.By the experiment of X ray double-crystal diffractometer and the contrast test of X ray spectrum practicality index, illustrate that the TAM crystal is better than PET to the detection performance of relevant spectral line.The attenuation ratio PET of high order diffraction is big, thereby ultimate analysis is had the better resisting interference ability.PET is good for TAM crystalline mechanical property ratio, and easy fracture is not convenient to make curved-crystal monochromator.The TAM crystalline growth velocity is fast, and growth cycle is short, and the yield rate height obtain the good large size single crystal of integrity than PET is easy, so the TAM crystal can replace the application of PET on X ray spectrum.
The top condition of TAM crystal growth is: prepare 60-40 ℃ saturated solution with analytically pure TAM reagent and redistilled water, long 1-2cm strip seed crystal with the paralleled by X axis direction, with automatic heat sink control cooling rate, can obtain 10 through 2 months growth cycles
6Mm
3Transparent large single crystal.
Claims (5)
1, a kind of crystalline material that is applicable to X-ray spectral analysis is characterized in that this crystal 2 d value is 8.78
(020) crystal face be its strongest diffraction surfaces, this crystal face has intact divisibility, its spectroscopic behaviour is better than the diffraction of (002) face of PET.
2, a kind of claim 1 described crystalline method that is used to grow, it is characterized in that with the aqueous solution cooling method growth used solvent is a water; Saturated solution is alkalescence; Small-crystalline that seed crystal employing nature is separated out or the strip crystal that is processed into paralleled by X axis; The growth temperature range from 60 ℃ to room temperature.
3, according to claim 2 described growing methods, it is characterized in that the most handy redistilled water of said solvent.
4, according to claim 2 described growing methods, it is characterized in that preparing the used TAM reagent of saturated solution is the analytical pure level.
5, a kind of monochromator of the x-ray spectrometer made from claim 1 described crystalline material is characterized in that the ultimate analysis wavelength region of this monochromator is identical with PET, and its spectroscopic behaviour is better than the PET monochromator.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN85107621.1A CN1003946B (en) | 1985-10-10 | 1985-10-10 | Trihydroxy methylaminomethane (tam) crystal, it's growth and application in x-rays-spectroscopy |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN85107621.1A CN1003946B (en) | 1985-10-10 | 1985-10-10 | Trihydroxy methylaminomethane (tam) crystal, it's growth and application in x-rays-spectroscopy |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN85107621A true CN85107621A (en) | 1986-09-03 |
| CN1003946B CN1003946B (en) | 1989-04-19 |
Family
ID=4795700
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN85107621.1A Expired CN1003946B (en) | 1985-10-10 | 1985-10-10 | Trihydroxy methylaminomethane (tam) crystal, it's growth and application in x-rays-spectroscopy |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1003946B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111678600A (en) * | 2020-08-10 | 2020-09-18 | 中国工程物理研究院激光聚变研究中心 | Hall crystal with flat response |
| CN112313505A (en) * | 2018-04-20 | 2021-02-02 | 奥图泰(芬兰)公司 | X-ray fluorescence analyzer and method for performing X-ray fluorescence analysis |
-
1985
- 1985-10-10 CN CN85107621.1A patent/CN1003946B/en not_active Expired
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112313505A (en) * | 2018-04-20 | 2021-02-02 | 奥图泰(芬兰)公司 | X-ray fluorescence analyzer and method for performing X-ray fluorescence analysis |
| CN111678600A (en) * | 2020-08-10 | 2020-09-18 | 中国工程物理研究院激光聚变研究中心 | Hall crystal with flat response |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1003946B (en) | 1989-04-19 |
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