CN106124540A - A kind of X-ray diffraction back pressure method of preferred orientation that can reduce is through sample board - Google Patents
A kind of X-ray diffraction back pressure method of preferred orientation that can reduce is through sample board Download PDFInfo
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- CN106124540A CN106124540A CN201610437037.XA CN201610437037A CN106124540A CN 106124540 A CN106124540 A CN 106124540A CN 201610437037 A CN201610437037 A CN 201610437037A CN 106124540 A CN106124540 A CN 106124540A
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- sample
- sample board
- micro slide
- board
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
- G01N23/2005—Preparation of powder samples therefor
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/30—Accessories, mechanical or electrical features
- G01N2223/312—Accessories, mechanical or electrical features powder preparation
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- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
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- Analysing Materials By The Use Of Radiation (AREA)
Abstract
The present invention relates to a kind of X-ray diffraction back pressure method of preferred orientation that can reduce through sample board, it is made up of sample board and micro slide, sample well is had on sample board, the surrounding of sample board tow sides sample well is coated with magnetisable material, described micro slide uses ferrous material, and micro slide can be pasted on sample board by the magnetisable material on sample board；The tow sides surface of polished of micro slide scribbles releasing material, prevents powder sample to be bonded on micro slide.During sample preparation, one piece of micro slide is inhaled on sample board front by magnetisable material, sample board overturns, then after powder sample being contained in sample well, then other a piece of micro slide is inhaled on the sample board back side, sample board is righted, finally takes off inhaling one piece of micro slide in sample board front, can test.The present invention can significantly decrease preferred orientation produced by sample surface region, thus reduces the change of diffracted ray relative intensity and the error that causes, it is thus achieved that X ray diffracting spectrum and test result more accurately.
Description
Technical field
The present invention relates to a kind of X-ray diffraction back pressure method of preferred orientation that can reduce through sample board.
Technical background
X-ray diffractometer is to utilize X-ray diffraction principle, accurately measures the crystal type of material, structure, texture and answers
Power, carries out material phase analysis, qualitative analysis and quantitative analysis accurately.It is widely used in metallurgy, oil, chemical industry, scientific research, aviation boat
My god, teaching, the field such as manufacture of materials.Sample board is one of important accessory of X-ray diffractometer, has direct shadow to test result
Ring.
The X-ray diffractometer method for making sample generally used all is difficult to avoid causing surface layer grain to have certain journey at sample plane
The preferred orientation of degree, the existence of preferred orientation has severely impacted the correct measurement of diffracted ray intensity.Use the most frequently used malleation
When legal system makees sample, the repeatability that diffracted intensity is measured is very poor, even can obtain the diffraction pattern that relative intensity size sequence is reverse
Spectrum.In order to reduce error, generally use through sample board and use back pressure method to be positioned on sample board by powder sample.But make
With time commonly through sample board, back pressure method is the most comparatively laborious, is typically clipped together with through sample board by microscope slide with clip,
Sample put in sample board and strike off, then being sealed with adhesive tape, then sample board is together overturn with microscope slide, take off folder
Son and microscope slide.Whole process is comparatively laborious, and easily makes a fault and cause sample preparation failure；Due to action of gravity, sample is also
Can sink causes test result to there is error.
Summary of the invention
It is an object of the invention to provide a kind of X-ray diffraction back pressure method that can reduce preferred orientation and pass through sample board,
Can significantly reduce preferred orientation produced by sample surface region, thus reduce the change of diffracted ray relative intensity and cause
Error, it is thus achieved that X ray diffracting spectrum and test result more accurately, make the back pressure convenient letter of method sample making course simultaneously
Single.
The X-ray diffraction back pressure method that can reduce preferred orientation that the present invention proposes is through sample board, by sample board and load
Thing sheet forms, and sample board has sample well, and the surrounding of sample board tow sides sample well is coated with magnetisable material, described loading
Sheet uses ferrous material, and micro slide can be pasted on sample board by the magnetisable material on sample board；Positive and negative the two of micro slide
Mirror polish rear surface scribbles releasing material, prevents powder sample to be bonded on micro slide.During sample preparation, one piece of micro slide is passed through magnetic
Material is inhaled on sample board front, and sample board overturns, after being then contained in sample well by powder sample, then by other a piece of load
Thing sheet is inhaled on the sample board back side, is righted by sample board, finally takes off inhaling one piece of micro slide in sample board front, Ji Kejin
Row test.
The present invention operation principle be: X-ray is linearly propagated, even if there is electric field and magnetic field, it can not be made to pass
Broadcasting direction to change, therefore, the magnetisable material on sample board does not interferes with the accuracy of test result.
The beneficial effects of the present invention is: 1. can significantly decrease preferred orientation produced by sample surface region, from
And reduce the change of diffracted ray relative intensity and the error that causes, it is thus achieved that X ray diffracting spectrum and test result more accurately；
2. using proposed by the invention when carrying out sample preparation through sample board, sample preparation is simple and convenient, the most error-prone.
Accompanying drawing explanation
Fig. 1 is the structural diagrams of the present invention；
The X ray diffracting spectrum of different method for making sample in Fig. 2 embodiment 1；
Label in figure: 1 is the first micro slide, 2 is sample board, and 3 is the second micro slide.
Detailed description of the invention
Combine accompanying drawing below by embodiment and further illustrate the present invention.
Embodiment 1: as it is shown in figure 1, described device is formed by through sample board 2 and two pieces of micro slides, sample board 2 has
Sample well, its two sides is covered with magnetisable material, it is possible to inhaled securely on sample board 2 by two pieces of non-sticky for irony micro slides；First
Micro slide 1 and the second micro slide 3 are irony, and surface of polished scribbles releasing material, prevents powder sample to be bonded on micro slide.
When sample preparation, the first micro slide 1 is inhaled on sample board 2 front, sample board 2 is overturn, powder sample is contained in sample well
After, second micro slide 3 is inhaled overleaf, sample board 2 is righted, take off inhaling the first micro slide 1 in sample board 2 front,
Can test.Use proposed by the invention when carrying out sample preparation through sample board, do not use the auxiliary such as clip and adhesive plaster to use
Product, sample preparation is simple and convenient, the most error-prone.
Test uses Ca (OH)2As test sample, its (011) family of crystal planes diffraction maximum shows obvious preferred orientation.
Test is taked three kinds of method for making sample: positive pressure method, use commonly pass through the back pressure method of sample board and use proposed by the invention
Back pressure method through sample board.By Rigaku Rigaku X-ray diffractometer (D/max2550VB3+/PC, Rigaku
International Corporation, Japan) with gathering X ray diffracting spectrum after different method for making sample sample preparations, wherein
Voltage x current is set as that 40kV/100mA, optical stop system slit are set as divergent slit=1 °, non-proliferation slit=1 °, receives slit
=0.3mm, sweep limits is set as 2θ=5-75 °, scanning speed is set as 2 °/min.According in the X ray diffracting spectrum recorded
(011) face and (001) face relative intensity compare its preferred orientation.Measured X ray diffracting spectrum is shown in Fig. 2, calculates gained
Relative intensity be shown in Table 1.
When (011) face (2θIt being 33.98 °) relative intensity is when being 100, as can be seen from Table 1: without preferentially in standard diagram
Orientation, (001) face (2θIt being 17.96 °) relative intensity is 71.8；Positive pressure method, common through sample board back pressure method and the present invention
Back pressure method (001) the face relative intensity of sample board is respectively 84.2,80.8 and 75.5.Result of the test shows that the present invention can show
Preferred orientation produced by the reduction sample surface region write, thus the mistake reducing the change of diffracted ray relative intensity and causing
Difference, can obtain X ray diffracting spectrum more accurately.
The X-ray diffraction relative intensity of the different method for making sample of table 1
Claims (1)
1. the X-ray diffraction back pressure method that can reduce preferred orientation passes through a sample board, is made up of sample board and micro slide,
It is characterized in that having on sample board sample well, the surrounding of sample board tow sides sample well is coated with magnetisable material, described load
Thing sheet uses ferrous material, and micro slide can be pasted on sample board by the magnetisable material on sample board；Micro slide positive and negative
Polishing both surfaces rear surface scribbles releasing material, prevents powder sample to be bonded on micro slide；During sample preparation, one piece of micro slide is passed through magnetic
Property material inhale on sample board front, sample board overturn, after then powder sample being contained in sample well, then will be the most a piece of
Micro slide is inhaled on the sample board back side, is righted by sample board, finally takes off inhaling one piece of micro slide in sample board front,
Test.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610437037.XA CN106124540A (en) | 2016-06-20 | 2016-06-20 | A kind of X-ray diffraction back pressure method of preferred orientation that can reduce is through sample board |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610437037.XA CN106124540A (en) | 2016-06-20 | 2016-06-20 | A kind of X-ray diffraction back pressure method of preferred orientation that can reduce is through sample board |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106124540A true CN106124540A (en) | 2016-11-16 |
Family
ID=57471029
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610437037.XA Pending CN106124540A (en) | 2016-06-20 | 2016-06-20 | A kind of X-ray diffraction back pressure method of preferred orientation that can reduce is through sample board |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106124540A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107228871A (en) * | 2017-07-21 | 2017-10-03 | 中国地质大学（武汉） | A kind of Portable X-ray analysis device |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2354134Y (en) * | 1998-10-29 | 1999-12-15 | 中国石化齐鲁石油化工公司 | Sample shelf for sample-changing device of X-ray diffractometer |
| CN101587035A (en) * | 2009-06-24 | 2009-11-25 | 中国铝业股份有限公司 | Sample preparing method for measuring superfine powder by X-ray diffraction instrument |
| CN202710490U (en) * | 2012-08-06 | 2013-01-30 | 深圳市禾苗分析仪器有限公司 | Magnetic adapter-type sample disk |
| CN205301032U (en) * | 2015-12-25 | 2016-06-08 | 中国石油天然气股份有限公司 | X X -ray diffraction sample frame of rule, isotactic polystyrene degree of crystallinity between survey |
-
2016
- 2016-06-20 CN CN201610437037.XA patent/CN106124540A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2354134Y (en) * | 1998-10-29 | 1999-12-15 | 中国石化齐鲁石油化工公司 | Sample shelf for sample-changing device of X-ray diffractometer |
| CN101587035A (en) * | 2009-06-24 | 2009-11-25 | 中国铝业股份有限公司 | Sample preparing method for measuring superfine powder by X-ray diffraction instrument |
| CN202710490U (en) * | 2012-08-06 | 2013-01-30 | 深圳市禾苗分析仪器有限公司 | Magnetic adapter-type sample disk |
| CN205301032U (en) * | 2015-12-25 | 2016-06-08 | 中国石油天然气股份有限公司 | X X -ray diffraction sample frame of rule, isotactic polystyrene degree of crystallinity between survey |
Non-Patent Citations (1)
| Title |
|---|
| 李波，郭永恒: "制样方法对XRD测定氧化铝中α-Al2O3含量的影响", 《耐火材料》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107228871A (en) * | 2017-07-21 | 2017-10-03 | 中国地质大学（武汉） | A kind of Portable X-ray analysis device |
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