CN208705253U - A kind of sealed sample frame suitable for environment sensitive material - Google Patents
A kind of sealed sample frame suitable for environment sensitive material Download PDFInfo
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- CN208705253U CN208705253U CN201821231076.5U CN201821231076U CN208705253U CN 208705253 U CN208705253 U CN 208705253U CN 201821231076 U CN201821231076 U CN 201821231076U CN 208705253 U CN208705253 U CN 208705253U
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Abstract
Sealed sample frame provided by the utility model includes cuboid ontology and groove, two halves disk and adhesive tape sealing film, the long 54mm of cuboid ontology, wide 35mm, thick 2mm, a long 20mm is opened up in the position away from sealed sample top of the trellis 13mm, wide 20mm, bilateral symmetry, depth are the groove of 1.5mm.Two semi-discs are arranged for loading environment sensitive sample, cuboid top and bottom portion of groove in groove, and corrugationless pastes adhesive tape sealing film on semi-disc, for sensitivity sample in sealed groove.When application analysis; in glove box under nitrogen protection; environment sensitive sample is uniformly filled and led up in sealed sample frame groove; formation sealed transparent film on semicircular ring is pasted into adhesive tape sealing film corrugationless; then X-ray diffraction analysis is carried out; because all incident X-rays and reflection X-ray are each perpendicular to adhesive tape surface, therefore back end signal is weaker, can obtain the X-ray diffraction analysis result of satisfactory environment sensitive sample.
Description
Technical field
The utility model design makes a kind of novel seal specimen holder, is specifically designed, makes one kind suitable for environment sensitive
The sealed sample frame of material X-ray diffraction analysis.
Background technique
Currently, having suitable for Rigaku company, Japan, Holland's Panalytical company X-ray diffractometer is eliminated or portion
Divide the commercialization sealed sample frame for eliminating back end signal interference.But Rigaku company, above-mentioned sealed sample frame Japan and Holland
Structure is complicated for the sealed sample frame that Panalytical company uses, and price is more expensive.
In general, during the X-ray diffraction measure of powdered sample, using a kind of conventional glass or aluminum specimen holder,
Firstly the need of under nitrogen protection, environment sensitive sample is added in specimen holder groove, it can be with being packed into after scraping blade flattens
Polybag (research method [J] petrochemical industry of Zhang Wanjing solid catalyst, 2001,30 (7): 576.) or transparent adhesive tape of sealing
Modified specimen holder (a kind of sealed sample frame [P] China for X-ray diffraction measure of Li Ruifeng, Wang Xiuhui with sealing
Patent: 204255712U, 2015-04-08.) in, on the sample stage of X-ray diffractometer, adjustment specimen holder is measured.On
State continuous mode to have the following disadvantages: 1. electrostatic interaction easily occurs for sample sack and sample room, and sample is easily unrestrained；2. analytical spectra
Contain stronger back end signal interference in figure, even if handling sealed plastic bag or adhesive tape using Chemical Measurement procedure of peak decomposing
Back end signal is also relatively difficult, causes its application range relatively limited, above-mentioned patent report its design, production sealed sample frame
Suitable for the polyolefin catalyst of middle and high angle, low angle sample analysis does not provide example.
In order to solve defect existing in the prior art, the utility model provides a kind of suitable for all environment sensitive materials
The sealed sample frame of X-ray diffraction analysis.
Utility model content
The purpose of this utility model is to provide a kind of sealed sample framves suitable for environment sensitive material, to reach system
Sample is easy, time saving, laborsaving, improves analysis efficiency, and can sufficiently meet wanting for the environmentally sensitive sample analysis technology of X-ray diffraction
It asks.
To achieve the goals above, the utility model provides a kind of sealed sample frame suitable for environment sensitive material.
In an embodiment, the sealed sample frame includes:
One cuboid ontology, length 54mm, width 35mm, thick 2mm；
One is used to uniformly fill and lead up the groove of environment sensitive sample, is provided on the cuboid ontology, and the groove
Length 20mm, width 20mm, depth 1.5mm, the length direction of the groove and the length direction of the cuboid ontology are same
To the width direction of the groove and the width direction of the cuboid ontology are in the same direction；Back gauge where the recess width
The distance of two short sides of the cuboid is respectively 13cm, 11cm, cuboid described in the back gauge where the length of the groove
The distances of two long sides be 7.5cm；
Two halves disk, including the first semi-disc and the second semi-disc, first semi-disc and second semi-disc are equal
It is vertically installed on the cuboid ontology and is spaced each other and be arranged in parallel, first semi-disc and second semi-disc are equal
The one side of the groove is set, wherein first semi-disc be vertically arranged along the width direction of the cuboid ontology and
Positioned at the top end of the cuboid ontology, second semi-disc is vertically arranged in the groove side far from first semi-disc
Along upper, the diameter of first semi-disc and second semi-disc is equal to the width of the cuboid ontology；
It is quick to scrape the whole environment of floating after the environment sensitive sample fills up groove naturally for adhesive tape sealing film
Feel sample surfaces, the adhesive tape sealing film corrugationless is pasted on two halfround bar slices quick to close the environment
Feel sample.
In an embodiment, the thickness of the two halves disk is 3mm.
In an embodiment, the sealed sample frame is metal or plastic material.
In an embodiment, the sealed sample frame material is stainless steel, aluminium alloy, chrome-plated metal material.
In an embodiment, the sealed sample frame be polyethylene, polypropylene, polytetrafluoroethylene (PTFE), polystyrene, ABS,
PEEK, nylon-6 material.
In an embodiment, the groove sample accommodating of the sealed sample frame is 0.6cm3。
In an embodiment, the sealed sample frame is integrally formed design.
The utility model has the beneficial effects that
(1) in the glove box of nitrogen protection, environment sensitive is added in the sealed sample frame sample groove through being dried
Sample does not have to apply external force, after sample fills up groove naturally, scrapes and smoothes out whole sample surfaces, be pasted into adhesive tape corrugationless
To close sample on two semi-discs.The adjustment sealed sample frame on powder x-ray diffraction sample stage, then carries out X-ray
Diffraction because back end signal is weaker, therefore can accurately obtain the true X-ray diffraction spectrogram of environment sensitive sample, the sealing sample
Product frame is primarily adapted for use in the moisture encountered in air, hydrolysis occurs for oxygen, oxidation, influences the environment sensitive material of measurement result,
Because sample to be tested can be isolated with oxygen, moisture in air, therefore extraneous factor can be eliminated in continuous mode to sample X-ray diffraction
The influence of measurement.
(2) realize that environment sensitive sample X-ray diffraction measure signal without back end signal interference, is avoided because of back end signal interference
Caused Data Post trouble.
(3) when carrying out subsequent X-ray diffraction analysis, acquired environment sensitive sample X-ray diffraction spectrum icon closes X
The requirement of x ray diffraction analysis x technology.
(4) the utility model specimen holder sample making course is easy, quick, and analysis efficiency can be improved；It is time saving, laborsaving simultaneously,
Analysis can sufficiently meet environment sensitive sample efficiently, quickly, the requirement of economic analysis, and can save and purchase commercialization sealed sample
Frame expense because can easily analyze all environment sensitive samples, therefore can be led in environment sensitive sample analysis
Domain promotes and applies.
Detailed description of the invention
Fig. 1 is the top view of the utility model sealed sample frame.
Fig. 2 is the left view of the utility model sealed sample frame.
Fig. 3 is the front view of the utility model sealed sample frame.
Fig. 4-1 is folded for the X-ray diffraction spectrogram for being repeated three times back end signal using the utility model sealed sample frame
Add display.
Fig. 4-2 is the X-ray diffraction spectrogram point that back end signal is repeated three times using the utility model sealed sample frame
From display.
Fig. 5-1 is to measure removed template method and the environment sensitive material through being dried using the utility model sealed sample frame
Expect the X-ray diffraction spectrogram Overlapping display of the X-ray diffraction spectrogram and the replication sample after the 4h of interval of SAPO-11.
Fig. 5-2 is to measure removed template method and the environment sensitive material through being dried using the utility model sealed sample frame
Expect that the X-ray diffraction spectrogram of SAPO-11 separates display with the X-ray diffraction spectrogram of the replication sample after the 4h of interval.
Fig. 6 is to measure removed template method using the utility model sealed sample frame and using common sample frame and through at dry
The X-ray diffraction spectrogram of the environment sensitive material SAPO-11 of reason separates display.
Wherein, appended drawing reference:
1 cuboid ontology
2 second semi-discs
3 first semi-discs
4 grooves
Specific embodiment
It elaborates below to the embodiments of the present invention, but not as the restriction to the utility model.
On the basis of the conventional sample frame of Rigaku company X-ray diffractometer measurement non-ambient sensitivity sample, structure is carried out
It improves, mainly uses 3D printing technique, select the material with processability, design, production sealed sample frame.
The utility model discloses a kind of sealed sample framves suitable for all environment sensitive material X-ray diffraction analysis.
It as shown in Figure 1-Figure 3, is the three-view diagram of the utility model sealed sample frame.The sealed sample frame includes a cuboid ontology, uses
In the groove, two halves disk and adhesive tape sealing film of uniformly filling and leading up environment sensitive sample, a length of 54mm of cuboid ontology,
Width is 35mm, thickness 2mm, opens up a long 20mm, wide 20mm in the position away from specimen holder top edge 13mm, bilateral symmetry,
Depth is the groove of 1.5mm.
The groove is for uniformly filling and leading up environment sensitive sample, and the length direction of the groove and the cuboid ontology
Length direction is in the same direction, and the width direction of the groove and the width direction of the cuboid ontology are in the same direction；The recess width institute
Back gauge described in the distance of two short sides of cuboid be respectively 13cm, 11cm, the back gauge where the length of the groove
The distance of two long sides of the cuboid is 7.5cm.In this present embodiment, sample groove volume is 0.6cm3, can sufficiently expire
Requirement of the sufficient X-ray diffraction to thickness of sample.
Two halves disk, including the first semi-disc and the second semi-disc, first semi-disc and second semi-disc are equal
It is vertically installed on the cuboid ontology and is spaced each other and be arranged in parallel, first semi-disc and second semi-disc are equal
The one side of the groove is set, wherein first semi-disc be vertically arranged along the width direction of the cuboid ontology and
Positioned at the top end of the cuboid ontology, second semi-disc is vertically arranged in the groove side far from first semi-disc
Along upper, the diameter of first semi-disc and second semi-disc is equal to the width of the cuboid ontology, i.e. diameter is equal
With specimen holder equivalent width, i.e. diameter is 35mm；Two halves disk and described this body by integral forming of cuboid design.Two halves disk
Size it is identical, and thickness is 3mm.
It is quick to scrape the whole environment of floating after the environment sensitive sample fills up groove naturally for adhesive tape sealing film
Feel sample surfaces, the adhesive tape corrugationless is pasted on two semi-discs to close the environment sensitive sample.
Two halves disk and described this body by integral forming of cuboid design, and entire sealed sample frame is integrally formed design.Sealed sample frame
Because all incident X-rays and reflection X-ray are each perpendicular to adhesive tape sealing film surface, therefore back end signal is weaker, applicable
Sample scope is wider, covers basic, normal, high angle, and X-ray diffraction analysis result is satisfactory.
The material of sealed sample frame is stainless steel, aluminium alloy, chrome-plated metal material or polyethylene, polypropylene, polytetrafluoroethyl-ne
Alkene, polystyrene, ABS, PEEK, nylon-6 material.The diameter of two halves disk is of same size with sealed sample frame, uses transparent adhesive tape
Band corrugationless, which is pasted on two semi-discs, forms sealing, it is ensured that incident ray direction all points to the center of circle, because all incidence X are penetrated
Line and reflection X-ray are each perpendicular to adhesive tape surface, therefore back end signal is weaker, and applicable sample scope is wider, cover it is low,
Middle and high angle, X-ray diffraction analysis result are satisfactory.
The utility model sealed sample frame, global shape meet Japan's Rigaku company X-ray diffractometer to sample used
The size requirement of product frame global shape, but it is not limited only to this, design philosophy is suitable for the X-ray diffractometer of all producers.If
Applied to other X-ray diffractometers, then the shape or size of sealed sample frame are needed according to different manufacturers X-ray diffractometer sample
The actual conditions of frame make corresponding dimension modifying.
Using sealed sample frame provided by the utility model, following operating process is taken:
Sample pretreatment:
In glove box under nitrogen protection, environment sensitive sample is placed in the agate mortar through being dried and is ground, led to
Mechanical lapping 30min often is needed, so that sample particle diameter is close to 10 μm.
Sample preparation:
In the glove box of nitrogen protection, environment sensitive sample is added in the sealed sample frame sample groove after being dried
Product do not have to apply external force, after sample fills up groove naturally, scrape and smooth out whole sample surfaces, be pasted onto two with adhesive tape corrugationless
Sample is closed on a semi-disc.
Sample analysis:
The adjustment sealed sample frame on powder x-ray diffraction sample stage, then under defined instrument operating condition into
Row X-ray diffraction measure.
Data processing:
To X ray diffracting data obtained, use the software of instrument configuration that correct data processing is carried out in accordance with regulations to obtain
It materialses the analysis result of middle each component.
Embodiment 1
Using the utility model sealed sample frame measurement three times back end signal X-ray diffraction spectrogram comparison, see Fig. 4-1,
Fig. 4-2.Fig. 4-1 is the X-ray diffraction spectrogram superposition that back end signal is repeated three times using the utility model sealed sample frame
Display；Fig. 4-2 is aobvious for the X-ray diffraction spectrogram separation for being repeated three times back end signal using the utility model sealed sample frame
Show.
Analysis the result shows that: its X-ray diffraction spectrogram can repeat, and back end signal is weaker.Illustrate using this reality
With novel seal specimen holder, the X-ray diffraction analysis of back end signal not interference environment sensitivity sample, analysis result is satisfactory.
Embodiment 2
Removed template method is measured using the utility model sealed sample frame and the environment sensitive material SAPO- through being dried
The X-ray diffraction spectrogram comparison of replication, is shown in Fig. 5-1, Fig. 5-2 after 11 and its interval 4h.Fig. 5-1 is practical new using this
Type sealed sample frame measure removed template method and the X-ray diffraction spectrogram of the environment sensitive material SAPO-11 through being dried and
The X-ray diffraction spectrogram Overlapping display of the replication sample after the 4h of interval；Fig. 5-2 is using the utility model sealed sample
Weight after frame measures the X-ray diffraction spectrogram of removed template method and the environment sensitive material SAPO-11 through being dried and is spaced 4h
Repetition measurement determines the X-ray diffraction spectrogram separation display of the sample.
Analysis the result shows that: its X-ray diffraction spectrogram can repeat.Illustrate to be made of the utility model sealed sample frame
Test piece good seal performance, analysis result it is satisfactory.
Embodiment 3
And using the utility model sealed sample frame and using common sample frame measurement removed template method be dried
The X-ray diffraction spectrogram of environment sensitive material SAPO-11 compares, see Fig. 6, Fig. 6 be using the utility model sealed sample frame with
Removed template method and the X-ray diffraction spectrogram of the environment sensitive material SAPO-11 through being dried are measured using common sample frame
Comparison, wherein curve a is to measure removed template method and the environment sensitive material SAPO-11 through being dried using common sample frame
X-ray diffraction spectrogram, curve b is to measure removed template method and ring through being dried using the utility model sealed sample frame
The X-ray diffraction spectrogram of border sensitive material SAPO-11.
Analysis the result shows that: its X-ray diffraction spectrogram is completely different.Sample is due to water suction in the test piece of commonsense method production
Generate new crystal (Al20H2Si2P18O80·16H2O)。
In addition the structure and performance test table of the sealed sample frame of the utility model and sealed sample frame in the prior art
It is as follows:
From the spectrogram comparative analysis test in embodiment 1, embodiment 2 and embodiment 3: being sealed using the utility model
The environmentally sensitive sample of specimen holder carries out sample preparation operation, and entire sample making course is easy, quick, analysis efficiency can be improved, and divide
Analysis result can satisfy environment sensitive sample quickly, accurate, economic analysis requirement.
Certainly, there are also other various embodiments for the utility model, in the feelings without prejudice to the spirit of the present invention and its essence
Under condition, those skilled in the art can make various corresponding changes and modifications according to the utility model, but these are corresponding
Change and modification, all should belong to the protection scope of the utility model the attached claims.
Claims (7)
1. a kind of sealed sample frame suitable for environment sensitive material, which is characterized in that the sealed sample frame includes:
One cuboid ontology, length 54mm, width 35mm, thick 2mm；
One, for uniformly filling and leading up the groove of environment sensitive sample, is provided on the cuboid ontology, and the length of the groove
20mm, width 20mm, depth 1.5mm, the length direction of the groove and the length direction of the cuboid ontology are in the same direction, institute
The width direction for stating groove and the width direction of the cuboid ontology are in the same direction；It is long described in back gauge where the recess width
The distance of two short sides of cube is respectively 13cm, 11cm, and two of cuboid described in the back gauge where the length of the groove are long
The distance on side is 7.5cm；
Two halves disk, including the first semi-disc and the second semi-disc, first semi-disc and second semi-disc are vertical
It is mounted on the cuboid ontology and is spaced each other and be arranged in parallel, first semi-disc and second semi-disc are respectively provided with
In the one side of the groove, wherein first semi-disc is vertically arranged and is located at along the width direction of the cuboid ontology
The top end of the cuboid ontology, second semi-disc are vertically arranged in the groove edge far from first semi-disc
On, the diameter of first semi-disc and second semi-disc is equal to the width of the cuboid ontology；
Adhesive tape sealing film is scraped after the environment sensitive sample fills up groove naturally and smoothes out the whole environment sensitive sample
The adhesive tape sealing film corrugationless is pasted on two semi-discs to close the environment sensitive sample by product surface
Product.
2. being suitable for the sealed sample frame of environment sensitive material as described in claim 1, which is characterized in that the two halves disk
Thickness be 3mm.
3. being suitable for the sealed sample frame of environment sensitive material as described in claim 1, which is characterized in that
The sealed sample frame is metal or plastic material.
4. being suitable for the sealed sample frame of environment sensitive material as claimed in claim 3, which is characterized in that
The sealed sample frame material is stainless steel, aluminium alloy, chrome-plated metal material.
5. being suitable for the sealed sample frame of environment sensitive material as claimed in claim 3, which is characterized in that the sealed sample
Frame is polyethylene, polypropylene, polytetrafluoroethylene (PTFE), polystyrene, ABS, PEEK, nylon-6 material.
6. being suitable for the sealed sample frame of environment sensitive material as claimed in claim 3, which is characterized in that the sealed sample
The groove sample accommodating of frame is 0.6cm3。
7. being suitable for the sealed sample frame of environment sensitive material as described in claim 1, which is characterized in that the sealed sample
Frame is integrally formed design.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201821231076.5U CN208705253U (en) | 2018-08-01 | 2018-08-01 | A kind of sealed sample frame suitable for environment sensitive material |
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| CN201821231076.5U CN208705253U (en) | 2018-08-01 | 2018-08-01 | A kind of sealed sample frame suitable for environment sensitive material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110887856A (en) * | 2019-11-04 | 2020-03-17 | 澳门大学 | Sample table for X-ray diffractometer, application of sample table and X-ray diffractometer |
| CN110887855A (en) * | 2019-11-04 | 2020-03-17 | 澳门大学 | X-ray diffraction sample cover, bearing mechanism and method for carrying out X-ray diffraction |
-
2018
- 2018-08-01 CN CN201821231076.5U patent/CN208705253U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110887856A (en) * | 2019-11-04 | 2020-03-17 | 澳门大学 | Sample table for X-ray diffractometer, application of sample table and X-ray diffractometer |
| CN110887855A (en) * | 2019-11-04 | 2020-03-17 | 澳门大学 | X-ray diffraction sample cover, bearing mechanism and method for carrying out X-ray diffraction |
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