CN107966463A - A kind of sample stage of X-ray diffractometer measurement fluid sample - Google Patents
A kind of sample stage of X-ray diffractometer measurement fluid sample Download PDFInfo
- Publication number
- CN107966463A CN107966463A CN201711290613.3A CN201711290613A CN107966463A CN 107966463 A CN107966463 A CN 107966463A CN 201711290613 A CN201711290613 A CN 201711290613A CN 107966463 A CN107966463 A CN 107966463A
- Authority
- CN
- China
- Prior art keywords
- crucible
- sample
- sample stage
- ray diffractometer
- mandril
- 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.)
- Granted
Links
Classifications
-
- 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
- G01N23/20025—Sample holders or supports therefor
- G01N23/20033—Sample holders or supports therefor provided with temperature control or heating means
Landscapes
- 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)
- Pathology (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
A kind of sample stage the invention discloses X-ray diffractometer with measurement fluid sample, including：The crucible furnace of temperature-adjustable, the silica crucible for holding sample and temperature-control heat couple, crucible furnace upper surface is recessed inwardly to be placed in groove equipped with a groove, silica crucible, and temperature-control heat couple insertion crucible furnace is adjusted with the temperature to crucible furnace.A kind of sample stage of present invention X-ray diffractometer measurement fluid sample, the temperature for the temperature-control heat couple control crucible furnace being inserted into crucible furnace, so as to which the silica crucible being opposite in crucible furnace heat simultaneously temperature control, solve the problems, such as necessary outer water flowing bath heating during current diffractometer test liquid, while widened the scope of heating.
Description
Technical field
The present invention relates to detection device technical field, more specifically, it is related to a kind of X-ray diffractometer measurement liquid
The sample stage of sample.
Background technology
Liquid has the architectural feature of shortrange order and longrange disorder.Its research method has two major classes, first, structure is straight
Measurement is connect, i.e., is measured using instrument；Another kind of is computer simulation method, obtains solution structure.It is it is worth noting that, single
One dependence molecular simulation cannot obtain real solution structure data, lack verification；Experimental data is still mark post, is to be managed
Think the basis of data.
But, can be direct in current measuring method so far without the proprietary instrument for solution structure measure
The accurate method for obtaining solution structure information is the experimental method based on scattering.The instrument that scattering method uses has the powder in laboratory
The X-ray scattering device of X-ray diffractometer or synchrotron radiation light source.The advantage of synchrotron radiation light source is that its brightness is big, steady
Qualitative height, high directivity, collimation are good, are that liquid-scattering generally acknowledged at present tests optimal light source, overcome experiment just
The brightness of room diffractometer is low, and stability is poor, and directionality is low, and diversity is strong, it is time-consuming the shortcomings of.But synchrotron radiation EXAFS (X-
Ray Absorption Fine Structure, X-ray absorption fine structure spectroscopy)) the larger atomic number system of general Study
Partial structurtes, and the overall structure of SR scattering methods research is limited smaller, the two mutual supplement with each other's advantages by atomic number.Certainly, X is penetrated
The application of line scattering method and synchrotron radiation method in liquid structure, opens the gate of liquid structure research.
But the whether X-ray scattering device of powder x-ray diffraction or synchrotron radiation light source, its supporting sample
Product groove (pond) is designed for solid sample, can not solve the problems, such as holding for fluid sample, especially temperature control problem, because
This, develops a kind of liquid-like sample platform and scatters it is particularly important that studying to solution, be particularly readily able to the sample of control fluid temperature
It is particularly important that platform.Patent CN201610023004.8 discloses a kind of liquid X-ray scattering sample cell, it includes setting reeded
Pond body and the open-topped sample cell being located in the pond body, equipped with water inlet pipe, outlet pipe, by water inlet pipe and water outlet pipe by thermostatted water
Water in bath introduces the interlayer that the pond body outer wall of sample cell is formed with pond body inner wall, carries out water-bath circulation, and then realize to liquid
The control of sample temperature, but the sample cell high-temperature part can only be controlled below bath temperature, and even if using oil bath pan, temperature is most
Height also can only achieve 300 DEG C, then helpless for the sample of higher temperature.When using transmission beam method test, also it is suitable only for few
The sample of number spy's low absorption coefficient, can not also test the sample of most higher absorption coefficients.Because transmission beam method
Fluid sample and film are very big to X-ray absorption, the scattering strength of detector measurement to meet statistical counting error 1%, it is necessary to
Data acquisition time it is longer, or even the time of one fluid sample of measurement need one week.To highly absorbing sample, transmission beam method collection
Less than scattering strength.Therefore, a kind of easy to operate not outer water flowing bath or oil bath heating are found and with higher heating model
The liquid-like sample platform enclosed just seems particularly urgent.
The content of the invention
In view of defect existing in the prior art, the sample the present invention provides a kind of X-ray diffractometer with measurement fluid sample
Sample platform, solves the problems, such as necessary outer water flowing bath heating during current diffractometer test liquid, while has widened the model of heating
Enclose.
In order to realize above-mentioned purpose, present invention employs following technical solution：
A kind of sample stage of X-ray diffractometer measurement fluid sample, including：The crucible furnace of temperature-adjustable, for containing
The silica crucible and temperature-control heat couple of setting-out product, the crucible furnace upper surface are recessed inwardly equipped with a groove, the silica crucible
It is placed in the groove, the temperature-control heat couple is inserted into the crucible furnace and is adjusted with the temperature to crucible furnace.
Further, the crucible furnace upper end edge is equipped with a notch, and the notch is used to match with X-ray diffractometer
Connection.
Further, the burner hearth is made of zirconia polycrystal fibrous material.
Further, further include the stove fixed seat arranged on the crucible furnace bottom, be respectively arranged on the stove fixed seat upper table
First support column and level meter in face, the adjusting part arranged on the stove fixed seat lower surface and be connected with the adjusting part with
The support device of the adjusting part is supported, first support column is equipped with multiple and is connected with the crucible furnace bottom to prop up
The crucible furnace is supportted, the level meter is used for the angle of inclination for measuring sample stage, and the adjusting part is used to incline to sample stage
Rake angle is adjusted.
Further, the support device includes height-adjustable elevating mechanism and the adjustable water on elevating mechanism
The level(l)ing mechanism that prosposition is put, surface of the level(l)ing mechanism away from the elevating mechanism are equipped with the second support column,
The top of second support column connects the adjusting part.
Further, the adjusting part includes the supporting table being connected with second support column and is uniformly arranged on the branch
Three supports supportted on platform adjust foot.
Further, the elevating mechanism includes bottom plate, liftable scissors mechanism and the control scissors mechanism lifting
The first adjusting rod, have two pairs on the scissors mechanism, wherein the scissors mechanism arranged on lower end be placed on the bottom plate and
Laterally wherein side is fixedly connected with the bottom plate, and two pairs of scissors mechanisms are up and down hingedly, and hinged place is horizontally connected with the
One cross bar and the second cross bar, first adjusting rod rotatably sequentially pass through the first cross bar and the second cross bar and stretch out the second horizontal stroke
Bar, first adjusting rod are threadedly coupled with the first cross bar, and one end that first adjusting rod stretches out second cross bar is equipped with
Prevent first adjusting rod from deviating from the first anti-falling piece of the second cross bar.
Further, two telescopic rods diagonally set are at least connected between the bottom plate and the level(l)ing mechanism,
The level(l)ing mechanism include fixed seat relatively-stationary with the telescopic rod top, in the fixed seat and relative to
The second adjusting rod that the horizontally slidable sliding stand of the fixed seat and the driving sliding stand are slided relative to the fixed seat,
Second support column is arranged on the upper surface of the sliding stand.
Further, the crucible furnace is equipped with second through hole coaxial with the groove, is worn in second through hole
There is a mandril, the silica crucible that the mandril is used to be placed in the groove ejects upwards.
Further, the bottom portion of groove is equipped with a quartzy backing plate for being used for support silica crucible, one end of the mandril
Through second through hole and with the quartzy pad contact, prevented with being equipped with one at the quartzy pad contact on the mandril
The convex shoulder that the mandril drops, the other end of the mandril stretch out second through hole, and the external part of the mandril, which is equipped with one, to be prevented
Only the second anti-falling piece of the mandril prolapse upwards, is equipped with elastic compression between second anti-falling piece and the crucible furnace bottom
Part, the elastic compression part is sheathed on the mandril and the both ends of elastic compression part abut the bottom and second of crucible furnace respectively
The surface of anti-falling piece.
A kind of sample stage of X-ray diffractometer measurement fluid sample provided by the invention, the temperature control being inserted into crucible furnace
Thermocouple controls the temperature of crucible furnace, so that the silica crucible being opposite in crucible furnace heat and temperature control, solves current
During diffractometer test liquid must the heating of outer water flowing bath the problem of, simultaneously because burner hearth have the temperature-adjustable of higher from
And the heated perimeter of warm table is widened；And sample stage position is adjusted by adjusting part and level(l)ing mechanism, pass through lifting
Mechanism adjusts sample stage whole height, and whole sample stage is compact-sized, easy to operate；At the same time bottom of furnace body be equipped with can freely up and down
Mobile mandril, it is convenient that crucible is picked and placeed so that in test, it is not necessary to replace sample stage, need to only take out in crucible furnace
Crucible can replace sample, simple to operate.
Brief description of the drawings
Fig. 1 is the structure diagram of the sample stage of X-ray diffractometer measurement fluid sample in the embodiment of the present invention；
Fig. 2 is the main structure diagram of the sample stage of X-ray diffractometer measurement fluid sample in the embodiment of the present invention；
Fig. 3 is the sectional view of A-A in Fig. 2；
Fig. 4 is the sample stage test kodalk for using X-ray diffractometer measurement fluid sample in the embodiment of the present invention
Scatter pattern under different temperatures；
Fig. 5 is the sample stage test kodalk for using X-ray diffractometer measurement fluid sample in the embodiment of the present invention
Different temperatures lower structure function collection of illustrative plates.
In figure：1. crucible furnace；11. furnace shell；12. burner hearth；13. bell；131. first through hole；14. groove；15. notch；
16. the second through hole；17. mandril；171. convex shoulder；172. second anti-falling pieces；173. elastic compression parts；18. quartzy backing plate；2. quartz
Crucible；3. temperature-control heat couple；4. stove fixed seat；5. the first support column；6. level meter；7. adjusting part；71. supporting table；72.
Support adjusts foot；8. support device；81. elevating mechanism；811. bottom plate；811-1. sides fixed plate；812. scissors mechanism；812a. the
One group of support feet；Second group of support feet of 812b.；The first cross bars of 812-1.；The second cross bars of 812-2.；813. first adjusting rods；
814. first anti-falling pieces；815. telescopic rod；82. level(l)ing mechanism；821. support plate；822. fixed seat；823. sliding stand；
824. second adjusting rods；825. the 3rd anti-falling pieces；83. the second support column；9. convex stent.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to the accompanying drawings and embodiments, it is right
The present invention is further described.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and do not have to
It is of the invention in limiting.
Referring to Fig. 1, a kind of sample stage of X-ray diffractometer measurement fluid sample provided in this embodiment, is adapted to X'
The powder x-ray diffractions such as Pert Pro, its sample stage include crucible furnace 1, the quartz for holding sample of temperature-adjustable
Temperature-control heat couple 3 on crucible 2 and insertion crucible furnace 1,1 upper surface of crucible furnace is recessed inwardly equipped with a groove 14, silica crucible 2
It is placed in groove 14, temperature-control heat couple 3 is inserted into crucible furnace 1 and by outside control with the temperature to the crucible furnace 1 being attached thereto
It is controlled, so that the temperature for the silica crucible 2 being opposite in crucible furnace 1 is adjusted.Preferably, in order to timely right
1 heat temperature raising of crucible furnace simultaneously has more preferable heat insulation effect to save resource, and crucible furnace 1 includes furnace shell 11, arranged on furnace shell 11
The adjustable burner hearth 12 of interior and temperature and the bell 13 being covered on furnace shell 11, then 12 upper surface of burner hearth be recessed inwardly to be formed it is recessed
Groove 14, place opposite with 14 position of groove is equipped with first through hole 131 on bell 13, and silica crucible 2 is placed in recessed through first through hole 131
In groove 14, temperature-control heat couple 3 through furnace shell 11 and be inserted into burner hearth 12 with the temperature to burner hearth 12 be controlled so as to fulfill
The temperature of opposed silica crucible 2 in the inner is adjusted.Further, in order to which more preferable diffracting effect, silica crucible 2 are placed in
Its top sides edge is flushed with the upper surface of bell 13 after groove 14.Preferably, sample stage heating furnace 12 uses heat-resisting material
It is made, preferably uses zirconia polycrystal fibrous material, using burner hearth 12 made of zirconia polycrystal fibrous material than passing
System furnace energy-saving 30%, temperature-controlled precision are ± 0.1 DEG C, and maximum temperature is up to 550 DEG C.Preferably, the diameter of burner hearth 12 can be according to reality
The sample stage placement space of border instrument is designed, correspondingly, the shape and size and silica crucible 2 of 12 inner groovy 14 of burner hearth
Size can be designed according to actual conditions.Wherein sample cell uses silica crucible, and temperature tolerance is strong, the sample cell design with
Diffractometer geometry matches, and can obtain the scattering strength of maximum, shortens time of measuring.
Wherein, temperature-control heat couple 3 is connected with exterior terminal, temperature-control heat couple 3 is controlled by exterior terminal, preferably
, exterior terminal is computer, and western nit intelligent temperature control software is preinstalled with computer, and multi-segment program control can be realized by the software
Temperature, programmable, automatic heating, insulation；Recordable, storage, show current or historical temperature curve, can also be entered by USB flash disk unloading
Computer, is easy to operate and control.
Referring to Fig. 1, the bottom of 1 bottom of crucible furnace is additionally provided with stove fixed seat 4, the surface opposite with crucible furnace 1 of stove fixed seat 4
On be respectively equipped with the first support column 5 and level meter 6, the first support column 5 is equipped with multiple and is connected with 1 bottom of crucible furnace to support
Crucible furnace 1, it is preferred that the first support column 5 is equipped with three and is uniformly distributed in the upper surface of stove fixed seat 4, it is preferred that three the
One support column, 5 one end is integrally formed with crucible furnace 1, and three 5 other ends of the first support column are secured by bolts in stove fixed seat 4
On.Wherein level meter 6 is used to measuring the angle of inclination of sample stage, level meter as a kind of common measurer for measuring low-angle by
Level meter 6, can directly be bolted to connection in the upper surface of stove fixed seat 4 by extensive use herein, referring to Fig. 3, preferably
, a groove being adapted with 6 shape of level meter can be set on the upper surface of stove fixed seat 4, level meter 6 is embedded in groove
It is spacing to be carried out to level meter 6, it will be understood that level meter 6 is connected with 4 horizontal parallel of stove fixed seat all the time.
Specifically, with reference to Fig. 1-Fig. 3, stove fixed seat 4 away from the surface of level meter 6 be equipped with to the angle of inclination of sample stage into
The adjusting part 7 of row adjustment；Preferably, adjusting part 7 is WidFin section instrument, and WidFin section instrument includes and the second support column
The supporting table 71 of 83 connections and uniformly three in supporting table 71, which support, adjusts foot 72, and three support tune are adjusted by rotating
Section foot 72 is adjusted the angle of inclination of sample stage with changing the height of support feet 72.Wherein each support adjusts foot 72
Adjustable tilt scope be upper and lower 5 °.
Specifically, referring to Fig. 3,7 bottom of adjusting part is connected with the support device 8 for being used to support adjusting part 7.Preferably
The height and horizontal level of support device 8 are adjustable, specifically, support device 8 includes height-adjustable elevating mechanism 81
With the level(l)ing mechanism 82 of the adjustable horizontal position on elevating mechanism 81, the upper end of level(l)ing mechanism 82 passes through bolt
One end of the second support column 83 is connected, the other end of the second support column 83 outwards has a protrusion, and supporting table 71 is equipped with and protrusion
The hole of connection is matched, the hole in supporting table 71 is connected so that adjusting part 7 is supported with raised on the second support column 83.
Specifically, with reference to Fig. 1 and Fig. 3, elevating mechanism 81 is cut including bottom plate 811, liftable scissors mechanism 812 and control
The first adjusting rod 813 that mechanism 812 lifts is pitched, has two pairs on scissors mechanism 812, the scissors mechanism 812 of wherein each pair is equal
It is made of the opposite X-frame in left and right two, for each X-frame by hingedly being formed among two boards or bar, each X-frame is equal up and down
There are two support feets, i.e., a pair of of scissors mechanism 812 includes four upper support feet and four lower support feets, two couple setting up and down cut
Pitch mechanism 812 to be hinged, wherein four lower support feets of upper scissors mechanism 812 and four upper support feets point of lower scissors mechanism 812
Yi Yiduiying not be hinged, wherein four lower support feets arranged on the scissors mechanism 812 of lower end are placed on bottom plate 811, wherein four
Lower of laterally opposite two of support feet is one group, that is, forms first group of support feet 812a and second group of support feet 812b, wherein the
One group of support feet 812a or second group of support feet 812b be fixed on 811 upper surface of bottom plate cause in 813 precession of the first adjusting rod or
A lateral movement of scissors mechanism 812, other side are fixed during person screws out.Preferably, for preferably fixation wherein one
Support feet is organized, side fixed plate 811-1 is fixed with bottom plate 811, side fixed plate 811-1 is equipped with two and is respectively arranged on opposite
Simultaneously one of which support feet is fixed with side fixed plate 811-1 for the both sides of X-frame, wherein, side fixed plate 811-1 can be with bottom plate
Side fixed plate 811-1, can be also provided with the L-shaped of two side walls by 811 Integral designs, wherein one side wall be bolted with
On bottom plate 811, other side wall is fixedly connected with one of which support feet, it is preferred that consolidates first group of support feet 812a with side
Fixed board 811-1 is fixed.Two pairs of 812 hinged places of scissors mechanism are horizontally connected with the first cross bar 812-1 and the second cross bar 812-2, its
In first the first adjusting rod of cross bar 813 rotatably sequentially pass through the first cross bar 812-1 and the second cross bar 812-2 and stretch out second
Cross bar 812-2, the first adjusting rod 813 are threadedly coupled with the first cross bar 812-1, and the first adjusting rod 813 stretches out the second cross bar 812-2
One end be equipped with prevent the first adjusting rod 813 deviate from the second cross bar 812-2 the first anti-falling piece 814.Screwing out the first adjusting rod
During 813, the first anti-falling piece 814 abuts the second cross bar 812-2, continues to screw out, and the first anti-falling piece 814 extrudes the second cross bar
812-2 and to close to the first cross bar 812-1 a lateral movement so that scissors mechanism 812 shrink height raise.Preferably, bottom plate
811 bottoms are connected with a convex supporting rack 9, can facilitate and the position of sample stage is moved, while convex supporting rack 9 also may be used
To be preferably connected with X-ray diffractometer.Preferably, the height setting that scissors mechanism 812 can adjust as needed is multipair, and
Multipair connection can refer to above-mentioned.
Specifically, referring to Fig. 1, be at least connected between bottom plate 811 and level(l)ing mechanism 82 two diagonally set it is flexible
Bar 815, it is preferred that the top of telescopic rod 815 is fixedly connected with support plate 821, support plate 821 with the flexible of telescopic rod 815 and
Position height changes, it is preferred that in order to which sample stage is more stable, telescopic rod 815 sets four, is respectively arranged on four of bottom plate 811
Angle, it will be understood that the scissors mechanism 812 of lifting is between support plate 821 and bottom plate 811, and in multiple telescopic rods 815 it
Between.
Specifically, with reference to Fig. 1 and Fig. 3, fixed seat 822 that level(l)ing mechanism 82 includes being fixedly arranged in support plate 821, set
In in fixed seat 822 and relative to the horizontally slidable sliding stand 823 of fixed seat 822 and driving sliding stand 823 relative to fixation
The second adjusting rod 824 that seat 822 slides, wherein fixed seat 822 are equipped with block close to one end of swing handle, which is equipped with
The hole for passing through the second adjusting rod 824, the side opposite with sliding stand 823 is equipped with groove, the second adjusting rod in fixed seat 822
824 grooves for passing through the hole on block and stretching into fixed seat 822 are simultaneously threadedly coupled with sliding stand 823, are passed through rotation second and are adjusted
Pole 824 horizontally advances or retreats (left and right horizontal moves in Fig. 3) so that the sliding stand 823 being threadedly coupled therewith is realized, at this time
Second adjusting rod 824 is not all the time in fixed seat 822 and horizontally moveable.Preferably, 824 water of the second adjusting rod in order to prevent
Translation is dynamic, on the one hand can be in the second adjusting rod 824 for stretching into groove on the both sides of block and be installed with obstruction second respectively
The snap ring that adjusting rod 824 moves horizontally, to prevent the second adjusting rod 824 from moving horizontally and deviate from fixed seat 822, on the other hand
The one end of the second adjusting rod 824 away from rotating handles can be caused to stretch out fixed seat 822, the 3rd anti-falling piece is set on external part
825, the 3rd anti-falling piece 825 prevents the second adjusting rod 824 from deviating from fixed seat 822.Slided it is appreciated that the second support column 83 is arranged on
The upper surface of platform 823.
Further, referring to Fig. 3, sample is picked and placeed and replaces in order to facilitate silica crucible.Crucible furnace 1 is equipped with and groove
14 the second coaxial through holes 16, are equipped with a mandril 17 in the second through hole 16, mandril 17 is used for the quartz being placed in groove 14
Crucible 2 ejects upwards.Preferably, 14 bottom of groove be equipped with one be used for support silica crucible 2 quartzy backing plate 18, the one of mandril 17
End is contacted through the second through hole 16 and with quartzy backing plate 18, and being equipped with one with quartzy 18 contact position of backing plate on mandril 17 prevents mandril 17
The convex shoulder 171 to drop, the other end of mandril 17 stretch out the second through hole 16, and the external part of mandril 17, which is equipped with one, prevents that mandril 17 is upward
Second anti-falling piece 172 of abjection, is equipped with elastic compression part 173, elastic compression part between 1 bottom of the second anti-falling piece 172 and crucible furnace
173 are sheathed on mandril 17 and the both ends of elastic compression part 173 abut bottom and the second anti-falling piece 172 of crucible furnace 1 respectively
Surface.Preferably, the second anti-falling piece 172 is nut, is threadedly coupled with mandril 17, it will be understood that the overall diameter of nut is more than the
The diameter of two through holes 16, elastic compression part 173 is ring spring, and the interior diameter of ring spring causes less than the overall diameter of nut
Ring spring is stuck in nut and crucible furnace bottom.
With reference to Fig. 1 and Fig. 3,1 upper end edge of crucible furnace is equipped with a notch 15, and notch 15 is used for and X-ray diffractometer
With connection.
Referring to Fig. 4 and Fig. 5, using the sample stage and X of a kind of X-ray diffractometer measurement fluid sample of embodiment itself
X ray diffractometer x tests kodalk, as can be seen that being tested when using the sample stage of embodiment kodalk from figure
When, high temperature causes interatomic bond distance to be increased slightly, and can obtain preferable result.
A kind of sample stage of X-ray diffractometer measurement fluid sample provided by the invention, the temperature control being inserted into crucible furnace
Thermocouple controls the temperature of crucible furnace, so that the silica crucible being opposite in crucible furnace heat and temperature control, solves current
During diffractometer test liquid must the heating of outer water flowing bath the problem of, simultaneously because burner hearth have the temperature-adjustable of higher from
And the heated perimeter of warm table is widened；And sample stage position is adjusted by adjusting part and level(l)ing mechanism, pass through lifting
Mechanism adjusts sample stage whole height, and whole sample stage is compact-sized, easy to operate；At the same time bottom of furnace body be equipped with can freely up and down
Mobile mandril, it is convenient that crucible is picked and placeed so that in test, it is not necessary to replace sample stage, need to only take out in crucible furnace
Crucible can replace sample, simple to operate.
It the above is only the embodiment of the application, it is noted that come for those skilled in the art
Say, on the premise of the application principle is not departed from, some improvements and modifications can also be made, these improvements and modifications also should be regarded as
The protection domain of the application.
Claims (10)
- A kind of 1. X-ray diffractometer sample stage of measurement fluid sample, it is characterised in that including：The crucible of temperature-adjustable Stove (1), the silica crucible (2) for holding sample and temperature-control heat couple (3), crucible furnace (1) upper surface, which is recessed inwardly, to be set There is a groove (14), the silica crucible (2) is placed in the groove (14), and the temperature-control heat couple (3) is inserted into the crucible Stove (1) is adjusted with the temperature to crucible furnace (1).
- 2. the X-ray diffractometer according to claim 1 sample stage of measurement fluid sample, it is characterised in that：The earthenware Crucible stove (1) upper end edge is equipped with a notch (15), and the notch (15) is used to match connection with X-ray diffractometer.
- 3. the X-ray diffractometer according to claim 2 sample stage of measurement fluid sample, it is characterised in that：The stove Thorax (12) is made of zirconia polycrystal fibrous material.
- 4. the sample stage of the X-ray diffractometer measurement fluid sample according to claim 1-3 any one, its feature exist In：Further include the stove fixed seat (4) arranged on the crucible furnace (1) bottom, be respectively arranged on the of stove fixed seat (4) upper surface One support column (5) and level meter (6), the adjusting part (7) arranged on stove fixed seat (4) lower surface and with the adjusting part (7) connect to support the support devices (8) of the adjusting part (7), first support column (5) be equipped with it is multiple and with it is described For the connection of crucible furnace (1) bottom to support the crucible furnace (1), the level meter (6) is used for the angle of inclination for measuring sample stage, institute Adjusting part (7) is stated to be used to be adjusted the angle of inclination of sample stage.
- 5. the X-ray diffractometer according to claim 4 sample stage of measurement fluid sample, it is characterised in that：The branch The level of support arrangement (8) adjustable horizontal position including height-adjustable elevating mechanism (81) and on elevating mechanism (81) Adjusting mechanism (82), surface of the level(l)ing mechanism (82) away from the elevating mechanism (81) are equipped with the second support column (83), the top of second support column (83) connects the adjusting part (7).
- 6. the X-ray diffractometer according to claim 5 sample stage of measurement fluid sample, it is characterised in that：The tune Section component (7) includes the supporting table (71) being connected with second support column (83) and is uniformly arranged in the supporting table (71) Three supports adjust foot (72).
- 7. the X-ray diffractometer according to claim 5 sample stage of measurement fluid sample, it is characterised in that：The liter Descending mechanism (81) include bottom plate (811), liftable scissors mechanism (812) and control that the scissors mechanism (812) lifts the One adjusting rod (813), has two pairs on the scissors mechanism (812), wherein the scissors mechanism (812) arranged on lower end is placed in institute State on bottom plate (811) and horizontal wherein side is fixedly connected with the bottom plate (811), two pairs of scissors mechanisms (812) are up and down It is hinged, and hinged place is horizontally connected with the first cross bar (812-1) and the second cross bar (812-2), first adjusting rod (813) can What is rotated sequentially passes through the first cross bar (812-1) and the second cross bar (812-2) and stretches out the second cross bar (812-2), and described first Adjusting rod (813) is threadedly coupled with the first cross bar (812-1), and first adjusting rod (813) stretches out the second cross bar (812- 2) one end is equipped with the first anti-falling piece (814) for preventing first adjusting rod (813) from deviating from the second cross bar (812-2).
- 8. the X-ray diffractometer according to claim 7 sample stage of measurement fluid sample, it is characterised in that：The bottom Two telescopic rods diagonally set (815), the horizontal tune are at least connected between plate (811) and the level(l)ing mechanism (82) Saving mechanism (82) is included with the relatively-stationary fixed seat in the telescopic rod (815) top (822), arranged on the fixed seat (822) Above and relative to the horizontally slidable sliding stand (823) of the fixed seat (822) and the driving sliding stand (823) relative to institute The second adjusting rod (824) of fixed seat (822) slip is stated, second support column (83) is arranged on the upper of the sliding stand (823) Surface.
- 9. the X-ray diffractometer according to claim 8 sample stage of measurement fluid sample, it is characterised in that：The earthenware Crucible stove (1) is equipped with second through hole (16) coaxial with the groove (14), and a mandril is equipped with second through hole (16) (17), the silica crucible (2) that the mandril (17) is used to be placed in the groove (14) ejects upwards.
- 10. the X-ray diffractometer according to claim 9 sample stage of measurement fluid sample, it is characterised in that：It is described recessed Groove (14) bottom is equipped with a quartzy backing plate (18) for being used for support silica crucible (2), and one end of the mandril (17) is described in Second through hole (16) is simultaneously contacted with the quartzy backing plate (18), is set on the mandril (17) with described quartzy backing plate (18) contact position There is a convex shoulder (171) for preventing the mandril (17) from dropping, the other end of the mandril (17) stretches out second through hole (16), The external part of the mandril (17) is equipped with second anti-falling piece (172) for preventing the mandril (17) prolapse upwards, and described second Elastic compression part (173) is equipped between anti-falling piece (172) and the crucible furnace (1) bottom, the elastic compression part (173) is sheathed on On the mandril (17) and the both ends of elastic compression part (173) abut bottom and the second anti-falling piece (172) of crucible furnace (1) respectively Surface.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711290613.3A CN107966463B (en) | 2017-12-08 | 2017-12-08 | Sample stage for measuring liquid sample for X-ray diffractometer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711290613.3A CN107966463B (en) | 2017-12-08 | 2017-12-08 | Sample stage for measuring liquid sample for X-ray diffractometer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107966463A true CN107966463A (en) | 2018-04-27 |
| CN107966463B CN107966463B (en) | 2020-07-31 |
Family
ID=61997955
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711290613.3A Active CN107966463B (en) | 2017-12-08 | 2017-12-08 | Sample stage for measuring liquid sample for X-ray diffractometer |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107966463B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109540942A (en) * | 2018-11-27 | 2019-03-29 | 东莞中子科学中心 | For scattering or the temperature-changeable automatic sample-changing device of diffraction experiment |
| CN110441337A (en) * | 2019-09-03 | 2019-11-12 | 丹东浩元仪器有限公司 | A kind of X-ray diffractometer multifunctional sample platform detection device |
| CN112432964A (en) * | 2020-12-16 | 2021-03-02 | 中国科学院广州能源研究所 | Sample holder for natural gas hydrate X-ray diffractometer test and application thereof |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62195545A (en) * | 1986-02-24 | 1987-08-28 | Rigaku Denki Kk | Sample heating furnace for single crystal x-ray diffracting device |
| CN1534289A (en) * | 2003-03-26 | 2004-10-06 | ������ѧ��ʽ���� | X-ray diffraction device |
| US20040258203A1 (en) * | 2002-06-17 | 2004-12-23 | Akihito Yamano | Crystal evaluating device |
| CN201025460Y (en) * | 2007-03-01 | 2008-02-20 | 鸿富锦精密工业（深圳）有限公司 | Bearing device |
| CN201783782U (en) * | 2010-08-11 | 2011-04-06 | 上海泰胜(东台)电力工程机械有限公司 | Wind energy tower barrel inside-welding flange vehicle |
| CN102298254A (en) * | 2011-08-16 | 2011-12-28 | 刘坎坎 | Concealed projector hanger |
| CN202305445U (en) * | 2010-04-28 | 2012-07-04 | 约旦河谷半导体有限公司 | Device for analyzing sample |
| CN102590253A (en) * | 2012-01-17 | 2012-07-18 | 中国科学院上海应用物理研究所 | High-temperature fused salt synchrotron radiation in-situ research device |
| CN204008510U (en) * | 2014-07-22 | 2014-12-10 | 河北工业大学 | A kind of θ-2 θ type X-ray diffraction device of measuring for liquid-scattering |
| CN104534879A (en) * | 2015-01-14 | 2015-04-22 | 中国科学院合肥物质科学研究院 | Method and minicrystal growing furnace for in-situ measurement of fusion method crystal growth microstructures through synchrotron radiation mu-XRD technology |
-
2017
- 2017-12-08 CN CN201711290613.3A patent/CN107966463B/en active Active
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62195545A (en) * | 1986-02-24 | 1987-08-28 | Rigaku Denki Kk | Sample heating furnace for single crystal x-ray diffracting device |
| US20040258203A1 (en) * | 2002-06-17 | 2004-12-23 | Akihito Yamano | Crystal evaluating device |
| CN1534289A (en) * | 2003-03-26 | 2004-10-06 | ������ѧ��ʽ���� | X-ray diffraction device |
| CN201025460Y (en) * | 2007-03-01 | 2008-02-20 | 鸿富锦精密工业（深圳）有限公司 | Bearing device |
| CN202305445U (en) * | 2010-04-28 | 2012-07-04 | 约旦河谷半导体有限公司 | Device for analyzing sample |
| CN201783782U (en) * | 2010-08-11 | 2011-04-06 | 上海泰胜(东台)电力工程机械有限公司 | Wind energy tower barrel inside-welding flange vehicle |
| CN102298254A (en) * | 2011-08-16 | 2011-12-28 | 刘坎坎 | Concealed projector hanger |
| CN102590253A (en) * | 2012-01-17 | 2012-07-18 | 中国科学院上海应用物理研究所 | High-temperature fused salt synchrotron radiation in-situ research device |
| CN204008510U (en) * | 2014-07-22 | 2014-12-10 | 河北工业大学 | A kind of θ-2 θ type X-ray diffraction device of measuring for liquid-scattering |
| CN104534879A (en) * | 2015-01-14 | 2015-04-22 | 中国科学院合肥物质科学研究院 | Method and minicrystal growing furnace for in-situ measurement of fusion method crystal growth microstructures through synchrotron radiation mu-XRD technology |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109540942A (en) * | 2018-11-27 | 2019-03-29 | 东莞中子科学中心 | For scattering or the temperature-changeable automatic sample-changing device of diffraction experiment |
| CN109540942B (en) * | 2018-11-27 | 2021-05-25 | 东莞中子科学中心 | Temperature-variable automatic sample changing device for scattering or diffraction experiment |
| CN110441337A (en) * | 2019-09-03 | 2019-11-12 | 丹东浩元仪器有限公司 | A kind of X-ray diffractometer multifunctional sample platform detection device |
| CN110441337B (en) * | 2019-09-03 | 2024-09-17 | 丹东浩元仪器有限公司 | Multifunctional sample stage detection device of X-ray diffractometer |
| CN112432964A (en) * | 2020-12-16 | 2021-03-02 | 中国科学院广州能源研究所 | Sample holder for natural gas hydrate X-ray diffractometer test and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107966463B (en) | 2020-07-31 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107966463A (en) | A kind of sample stage of X-ray diffractometer measurement fluid sample | |
| US9457350B2 (en) | Rack for use with a temperature controlled bath, and a related method | |
| JP2024520237A (en) | Method for programmatic freezing of cells, system and device therefor | |
| US6329645B2 (en) | Apparatus for dampening standing wave pattern generation in microwave oven | |
| CN107941464A (en) | A kind of head-up display visual field testboard | |
| CN108827814B (en) | Simulate dry method rubber grain and asphalt grouting and cubical expansivity measurement device and method | |
| CN106091905A (en) | A kind of soil sample multidirectional humidification deformation measuring device and measuring method | |
| CN205388580U (en) | Sample pool for liquid X-ray scattering | |
| CN201622252U (en) | Micro-focus X-ray phase contrast imaging experimental platform | |
| CN202750560U (en) | Water maze device for water temperature constant temperature control | |
| Poplawsky et al. | Mixed layer development in a double-diffusive, thermohaline system | |
| CN207689396U (en) | A kind of temperature loading device for neutron scattering experiment | |
| CN205484234U (en) | Pesticide residue detection device | |
| CN208810109U (en) | A kind of thermostat water bath | |
| CN211329450U (en) | Can regulate and control and prevent shaking water bath | |
| CN205786541U (en) | A kind of pharmaceutical analysis apparatus | |
| CN209372634U (en) | A kind of attemperator for pitch cloth viscosity apparatus | |
| CN208476725U (en) | fluid viscosity coefficient testing device | |
| CN208568112U (en) | A kind of photovoltaic module temperature coefficient test macro of angle adjustable | |
| CN206716011U (en) | A kind of rack for test tube | |
| CN206642742U (en) | A kind of thermostatical circulating water bath system | |
| CN115790840B (en) | Device and method for testing illumination of operation shadowless lamp | |
| CN210923710U (en) | Urine trace element reagent detection device | |
| CN110186809A (en) | A kind of novel frozen soil rheometer | |
| CN214389905U (en) | Horizontal oscillator for chemistry experiments |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |