CN107966463B - Sample stage for measuring liquid sample for X-ray diffractometer - Google Patents
Sample stage for measuring liquid sample for X-ray diffractometer Download PDFInfo
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- CN107966463B CN107966463B CN201711290613.3A CN201711290613A CN107966463B CN 107966463 B CN107966463 B CN 107966463B CN 201711290613 A CN201711290613 A CN 201711290613A CN 107966463 B CN107966463 B CN 107966463B
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- 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
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Abstract
The invention discloses a sample stage for measuring a liquid sample for an X-ray diffractometer, which comprises: but temperature regulation's crucible stove, be used for holding the quartz crucible and the accuse temperature thermocouple of sample, crucible stove upper surface is equipped with a recess inwards sunken, and in the recess was arranged in to quartz crucible, the temperature thermocouple inserted the crucible stove in order to adjust the temperature of crucible stove. The sample stage for measuring the liquid sample for the X-ray diffractometer controls the temperature of the crucible furnace by the temperature control thermocouple inserted into the crucible furnace, thereby heating and controlling the temperature of the quartz crucible arranged in the crucible furnace, solving the problem that the current diffractometer needs to be heated by a water bath pot through the outside when testing the liquid, and simultaneously widening the heating range.
Description
Technical Field
The invention relates to the technical field of detection equipment, in particular to a sample table for measuring a liquid sample for an X-ray diffractometer.
Background
Liquids have structural features that are short-range ordered and long-range disordered. The research methods are divided into two categories, one is direct measurement of the structure, namely measurement is carried out by adopting an instrument; the other is a computer simulation method, which obtains the solution structure. It is worth noting that the true solution structure data cannot be obtained by relying on molecular simulation alone, and the verification is lacked; the experimental data are still benchmarks and are the basis for obtaining ideal data.
However, no special instrument for solution structure determination exists so far, and in the current measurement method, the method capable of directly and accurately obtaining solution structure information is an experimental method based on scattering. The scattering method uses a laboratory powder X-ray diffractometer or an X-ray scattering device which is a synchrotron radiation light source. The synchrotron radiation light source has the advantages of high brightness, high stability, strong directivity and good parallelism, is the most ideal light source for the liquid scattering experiment acknowledged at present, and just overcomes the defects of low brightness, poor stability, low directivity, strong divergence, time consumption and the like of a laboratory diffractometer. However, the X-Ray Absorption Fine Structure (X-Ray Absorption Fine Structure) of the synchrotron radiation is generally used to study the local Structure of a system with a larger atomic number, while the overall Structure studied by the SR scattering method is less limited by the atomic number, and the advantages of the two are complementary. The use of X-ray scattering and synchrotron radiation in liquid structures has undoubtedly opened the door to the study of liquid structures.
However, no matter the powder X-ray diffractometer or the X-ray scattering device of the synchrotron radiation light source, the sample tank (cell) matched with the device is designed for the solid sample, and the problem of containing the liquid sample, especially the temperature control problem, cannot be solved, so that the development of a liquid sample platform is particularly important for the research of solution scattering, and particularly the development of a sample platform capable of easily controlling the liquid temperature is particularly important. Patent CN201610023004.8 discloses a liquid X-ray scattering sample cell, it is including establishing the cell body of recess and establishing at open-top's in the cell body sample cell is equipped with inlet tube, outlet pipe, introduces the intermediate layer that the cell body outer wall and the cell body inner wall formed of sample cell with the water bath of thermostatic control through business turn over water pipe, carries out the water bath circulation, and then realizes the control to liquid sample temperature, but this sample cell high temperature part can only be controlled below the water bath temperature, even adopt the oil bath pot, the temperature can only reach 300 ℃ at the highest, then can not do nothing to the sample of higher temperature. When the transmission method is used for testing, the method is only suitable for a few samples with extremely low absorption coefficients, and the method cannot be used for testing most samples with higher absorption coefficients. Because the liquid sample and the film of the transmission method have great absorption to X-rays, the scattering intensity measured by the detector needs to meet the statistical counting error of 1 percent, the required data acquisition time is longer, and even the time for measuring one liquid sample needs one week. For highly absorbing samples, no scattering intensity was collected by transmission. Therefore, it is very urgent to find a liquid sample stage which is convenient to operate, does not need to be heated by an external water bath or an oil bath and has a higher heating range.
Disclosure of Invention
In view of the defects in the prior art, the invention provides a sample stage for measuring a liquid sample for an X-ray diffractometer, which solves the problem that the existing diffractometer needs to be heated by an external water bath pot when testing liquid, and widens the heating range.
In order to achieve the purpose, the invention adopts the following technical scheme:
a sample stage for measuring a liquid sample for an X-ray diffractometer, comprising: but temperature regulation's crucible stove, be used for holding the quartz crucible and the accuse temperature thermocouple of sample, crucible stove upper surface is inwards sunken to be equipped with a recess, quartz crucible arranges in the recess, accuse temperature thermocouple inserts the crucible stove is adjusted with the temperature to the crucible stove.
Furthermore, a notch is arranged at the edge of the upper end of the crucible furnace and is used for being connected with an X-ray diffractometer in a matching mode.
Further, the hearth is made of a zirconia polycrystalline fiber material.
Further, still including locating the stove fixing base of crucible stove bottom, locate respectively the first support column and the spirit level of stove fixing base upper surface, locate the adjusting part of stove fixing base lower surface and with the adjusting part is connected in order to support adjusting part's strutting arrangement, first support column be equipped with a plurality ofly and all with crucible stove bottom is connected in order to support the crucible stove, the spirit level is used for measuring the inclination of sample platform, adjusting part is used for adjusting the inclination of sample platform.
Furthermore, the supporting device comprises a lifting mechanism with adjustable height and a horizontal adjusting mechanism arranged on the lifting mechanism and capable of adjusting the horizontal position, a second supporting column is arranged on the surface of the horizontal adjusting mechanism far away from the lifting mechanism, and the top end of the second supporting column is connected with the adjusting assembly.
Furthermore, the adjusting component comprises a supporting platform connected with the second supporting column and three supporting adjusting feet uniformly arranged on the supporting platform.
Further, elevating system includes the scissors mechanism and the control of bottom plate, liftable scissors the first regulation pole that the fork mechanism goes up and down, scissors the mechanism and be equipped with two pairs from top to bottom, wherein locate the lower extreme scissors the mechanism and arrange in on the bottom plate and horizontal wherein one side with bottom plate fixed connection, two pairs scissors the fork mechanism and articulate from top to bottom, and articulated department transverse connection has first horizontal pole and second horizontal pole, first regulation pole is rotatable to pass first horizontal pole and second horizontal pole in proper order and stretch out the second horizontal pole, first regulation pole and first horizontal pole threaded connection, first regulation pole stretches out the one end of second horizontal pole is equipped with prevents first regulation pole is deviate from the first anticreep piece of second horizontal pole.
Furthermore, at least two telescopic rods arranged diagonally are connected between the bottom plate and the horizontal adjusting mechanism, the horizontal adjusting mechanism comprises a fixed seat fixed relative to the top end of the telescopic rod, a sliding table arranged on the fixed seat and capable of horizontally sliding relative to the fixed seat, and a second adjusting rod driving the sliding table to slide relative to the fixed seat, and the second supporting column is arranged on the upper surface of the sliding table.
Furthermore, a second through hole coaxial with the groove is formed in the crucible furnace, a push rod penetrates through the second through hole, and the push rod is used for pushing the quartz crucible arranged in the groove upwards.
Further, recess bottom is equipped with a quartz backing plate that is used for bearing quartz crucible, the one end of ejector pin passes the second through-hole and with the contact of quartz backing plate, on the ejector pin with quartz backing plate contact department is equipped with one and prevents the convex shoulder that the ejector pin dropped, the other end of ejector pin stretches out the second through-hole, the end that stretches out of ejector pin is equipped with one and prevents the second anticreep piece that the ejector pin upwards deviate from, the second anticreep piece with be equipped with the elastic compression piece between crucible furnace bottom, the elastic compression piece cover is located on the ejector pin and the both ends of elastic compression piece are the surface of butt crucible furnace's bottom and second anticreep piece respectively.
According to the sample stage for measuring the liquid sample for the X-ray diffractometer, the temperature control thermocouple inserted into the crucible furnace controls the temperature of the crucible furnace, so that a quartz crucible arranged in the crucible furnace is heated and controlled, the problem that a water bath kettle needs to be filled with water to heat when the liquid is measured by the existing diffractometer is solved, and meanwhile, the heating range of the heating stage is widened due to the fact that a hearth has higher adjustable temperature; the position of the sample table is adjusted through the adjusting assembly and the horizontal adjusting mechanism, the overall height of the sample table is adjusted through the lifting mechanism, and the whole sample table is compact in structure and convenient to operate; simultaneously, the bottom of the furnace body is provided with an ejector rod capable of freely moving up and down, so that the crucible can be conveniently taken and placed, the sample platform does not need to be replaced during testing, the crucible in the crucible furnace only needs to be taken out, and the sample can be replaced, and the operation is simple and convenient.
Drawings
FIG. 1 is a schematic structural diagram of a sample stage for measuring a liquid sample for an X-ray diffractometer according to an embodiment of the present invention;
FIG. 2 is a schematic front view of a sample stage for measuring a liquid sample for an X-ray diffractometer according to an embodiment of the present invention;
FIG. 3 is a cross-sectional view A-A of FIG. 2;
FIG. 4 is a scattering diagram of sodium metaborate measured by an X-ray diffractometer at different temperatures using a sample stage for measuring a liquid sample according to an embodiment of the present invention;
FIG. 5 is a structural function diagram of sodium metaborate measured by an X-ray diffractometer using a sample stage for measuring a liquid sample in the embodiment of the present invention at different temperatures.
In the figure: 1. a crucible furnace; 11. a furnace housing; 12. a hearth; 13. a furnace cover; 131. a first through hole; 14. a groove; 15. a notch; 16. a second through hole; 17. a top rod; 171. a shoulder is formed; 172. a second drop prevention member; 173. a resilient compression member; 18. a quartz backing plate; 2. a quartz crucible; 3. a temperature control thermocouple; 4. a furnace fixing seat; 5. a first support column; 6. a level gauge; 7. an adjustment assembly; 71. a support table; 72. supporting the adjusting foot; 8. a support device; 81. a lifting mechanism; 811. a base plate; 811-1. side fixing plate; 812. a scissor mechanism; 812a, a first set of support legs; 812b. a second set of support feet; 812-1. a first cross-bar; 812-2. a second cross bar; 813. a first adjusting lever; 814. a first drop prevention member; 815. a telescopic rod; 82. a horizontal adjustment mechanism; 821. a support plate; 822. a fixed seat; 823. a sliding table; 824. a second adjusting lever; 825. a third anti-stripping element; 83. a second support column; 9. a convex bracket.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Referring to fig. 1, the sample stage for measuring a liquid sample for an X-ray diffractometer provided by this embodiment is suitable for a powder X-ray diffractometer such as X' Pert Pro, and includes a crucible furnace 1 capable of adjusting temperature, a quartz crucible 2 for holding a sample, and a temperature control thermocouple 3 inserted into the crucible furnace 1, wherein a groove 14 is recessed inward on an upper surface of the crucible furnace 1, the quartz crucible 2 is placed in the groove 14, and the temperature control thermocouple 3 is inserted into the crucible furnace 1 and controls the temperature of the crucible furnace 1 connected thereto by external control, so as to adjust the temperature of the quartz crucible 2 placed in the crucible furnace 1. Preferably, in order to heat and raise the temperature of the crucible furnace 1 in time and have a better heat preservation effect to save resources, the crucible furnace 1 comprises a furnace shell 11, a temperature-adjustable furnace 12 arranged in the furnace shell 11 and a furnace cover 13 covering the furnace shell 11, the upper end surface of the furnace 12 is recessed inwards to form a groove 14, a first through hole 131 is arranged at a position opposite to the groove 14 on the furnace cover 13, the quartz crucible 2 penetrates through the first through hole 131 and is arranged in the groove 14, and the temperature control thermocouple 3 penetrates through the furnace shell 11 and is inserted into the furnace 12 to control the temperature of the furnace 12 so as to adjust the temperature of the quartz crucible 2 arranged in the furnace. Further, for better diffraction effect, the quartz crucible 2 is placed in the recess 14 with its top edge flush with the upper end surface of the lid 13. Preferably, the sample table heating hearth 12 is made of high-temperature resistant materials, preferably zirconia polycrystalline fiber materials, the hearth 12 made of the zirconia polycrystalline fiber materials saves energy by 30 percent compared with a traditional electric furnace, the temperature control precision is +/-0.1 ℃, and the highest temperature reaches 550 ℃. Preferably, the diameter of the hearth 12 can be designed according to the placing space of the sample stage of the actual instrument, and correspondingly, the shape and the size of the groove 14 in the hearth 12 and the size of the quartz crucible 2 can be designed according to the actual situation. The sample cell adopts a quartz crucible, has strong temperature resistance, is designed to be matched with the geometry of a diffractometer, can obtain the maximum scattering intensity and shortens the measurement time.
The temperature control thermocouple 3 is connected with an external terminal, the temperature control thermocouple 3 is controlled by the external terminal, preferably, the external terminal is a computer, and West Nite intelligent temperature control software is pre-installed in the computer, and multi-section program temperature control, programming, automatic temperature rise and heat preservation can be realized through the software; the current or historical temperature curve can be recorded, stored and displayed, and can also be transferred into a computer through a USB flash disk, so that the operation and control are easy.
Referring to fig. 1, the bottom of crucible furnace 1 bottom still is equipped with stove fixing base 4, stove fixing base 4 is equipped with first support column 5 and spirit level 6 respectively on the surface with crucible furnace 1 is relative, first support column 5 is equipped with a plurality ofly and all is connected in order to support crucible furnace 1 with crucible furnace 1 bottom, preferentially, first support column 5 is equipped with three and evenly distributed in the upper surface of stove fixing base 4, preferentially, 5 one end of three first support column and 1 an organic whole of crucible furnace are formed, the other one end of three first support column 5 is passed through the bolt fastening on stove fixing base 4. Wherein spirit level 6 is used for measuring the inclination of sample platform, and the spirit level has been widely used as the commonly used measuring tool of measuring the small angle, and here can be directly with spirit level 6 through bolt fixed connection in the upper surface of stove fixing base 4, see figure 3, preferably, can set up a recess that suits with 6 shapes of spirit level on the upper surface of stove fixing base 4, inlay spirit level 6 in the recess in order to carry on spacingly to spirit level 6, can understand, spirit level 6 is connected with 4 horizontal parallel of stove fixing base all the time.
Specifically, with reference to fig. 1 to 3, an adjusting assembly 7 for adjusting the inclination angle of the sample stage is arranged on the surface of the furnace fixing seat 4 away from the level 6; preferably, the adjusting component 7 is a horizontal micro-adjuster, the horizontal micro-adjuster comprises a supporting base 71 connected with the second supporting column 83 and three supporting adjusting feet 72 uniformly arranged on the supporting base 71, and the three supporting adjusting feet 72 are adjusted by rotating to change the height of the supporting feet 72 so as to adjust the inclination angle of the sample stage. Wherein the adjustable inclination of each support adjustment foot 72 ranges up and down by 5 °.
Specifically, referring to fig. 3, a supporting device 8 for supporting the adjusting assembly 7 is connected to the bottom of the adjusting assembly 7. The height and the horizontal position of the preferable supporting device 8 can be adjusted, specifically, the supporting device 8 comprises a height-adjustable lifting mechanism 81 and a horizontal adjusting mechanism 82 arranged on the lifting mechanism 81 and capable of adjusting the horizontal position, the upper end of the horizontal adjusting mechanism 82 is connected with one end of a second supporting column 83 through a bolt, the other end of the second supporting column 83 is outwards provided with a bulge, a hole matched and connected with the bulge is formed in the supporting table 71, and the hole in the supporting table 71 is connected with the bulge in the second supporting column 83 so that the adjusting component 7 can be supported.
Specifically, with reference to fig. 1 and 3, a lifting mechanism 81 comprises a base plate 811, a liftable scissors mechanism 812 and a first adjusting rod 813 for controlling the lifting of the scissors mechanism 812, two pairs of scissors mechanisms 812 are arranged above and below, each pair of scissors mechanism 812 consists of a left and a right opposite X-shaped frames, each X-shaped frame is formed by hinging two plates or rods, each X-shaped frame is provided with two support legs above and below, namely, a pair of scissors mechanism 812 comprises four upper support legs and four lower support legs, two pairs of scissors mechanisms 812 arranged above and below are hinged, four lower support legs of the upper scissors mechanism 812 and four upper support legs of the lower scissors mechanism 812 are respectively hinged in a one-to-one correspondence manner, four lower support legs of the scissors mechanism 812 arranged at the lower end are arranged on the base plate 811, wherein two laterally opposite support legs 812a are a set, namely, a first set of support legs 812a and a second set of support legs 812b, wherein the first set of the support legs 812a or the second set of the support legs 812a set of the first set 812a set is fixed on the upper surface of the base plate 811, a first set such that the support legs 812a cross bar 812a first set can be connected with a fixed on the side wall 811 of a first set by screwing in a cross bar 811, and a set of a first set as a cross bar 812, and a set to a set, a set for enabling a set of a set to be capable of a cross bar 811, and a set to be capable of a cross bar 811, and a set to be capable of extending from a cross bar 811, and a set to be capable of a set, and a set to be capable of extending from a set, and a set to be capable of extending from a set to a cross bar 811, and a set to be capable of extending from a set to a set, and to a set to a cross bar 811, and a set to a set, and a set to be capable of a set, and a set to a set of supporting plate 811, and a cross bar 811, and a set of a set.
Specifically, referring to fig. 1, at least two diagonally arranged telescopic rods 815 are connected between the bottom plate 811 and the horizontal adjustment mechanism 82, preferably, a support plate 821 is fixedly connected to a top end of the telescopic rod 815, and the position and height of the support plate 821 are changed along with the extension and contraction of the telescopic rod 815, preferably, four telescopic rods 815 are arranged at four corners of the bottom plate 811 for more stable sample platform, and it can be understood that the lifting scissor mechanism 812 is located between the support plate 821 and the bottom plate 811 and between the plurality of telescopic rods 815.
Specifically, referring to fig. 1 and 3, the horizontal adjustment mechanism 82 includes a fixing base 822 fixedly disposed on the supporting plate 821, a sliding table 823 disposed on the fixing base 822 and capable of horizontally sliding with respect to the fixing base 822, and a second adjustment lever 824 driving the sliding table 823 to slide with respect to the fixing base 822, wherein a stopper is disposed at an end of the fixing base 822 close to the rotating handle, a hole is disposed on the stopper, through which the second adjustment lever 824 passes, a groove is disposed on a side of the fixing base 822 opposite to the sliding table 823, the second adjustment lever 824 passes through the hole on the stopper and extends into the groove on the fixing base 822 and is in threaded connection with the sliding table 823, the sliding table 823 in threaded connection with the second adjustment lever 824 is horizontally moved forward or backward (horizontally moved left and right in fig. 3) by rotating the second adjustment lever 824, and at this time, the second adjustment. Preferably, in order to prevent the second adjustment lever 824 from moving horizontally, on one hand, snap rings for blocking the second adjustment lever 824 from moving horizontally are fixedly disposed on two sides of the second adjustment lever 824 extending into the groove, which are located at the stop, respectively, so as to prevent the second adjustment lever 824 from moving horizontally and coming off the fixing seat 822, on the other hand, one end of the second adjustment lever 824, which is far away from the rotating handle, may also extend out of the fixing seat 822, a third anti-disengaging member 825 is disposed on the extending end, and the third anti-disengaging member 825 prevents the second adjustment lever 824 from coming off the fixing seat 822. It is understood that the second support post 83 is provided on the upper surface of the slide table 823.
Further, referring to fig. 3, the handling and the replacement of the sample are facilitated for the quartz crucible. The crucible furnace 1 is provided with a second through hole 16 coaxial with the groove 14, a mandril 17 penetrates through the second through hole 16, and the mandril 17 is used for pushing the quartz crucible 2 arranged in the groove 14 upwards. Preferably, a quartz backing plate 18 for supporting the quartz crucible 2 is arranged at the bottom of the groove 14, one end of the ejector rod 17 penetrates through the second through hole 16 and contacts with the quartz backing plate 18, a convex shoulder 171 for preventing the ejector rod 17 from falling is arranged at the contact position of the ejector rod 17 and the quartz backing plate 18, the other end of the ejector rod 17 extends out of the second through hole 16, a second anti-falling part 172 for preventing the ejector rod 17 from falling off upwards is arranged at the extending end of the ejector rod 17, an elastic compression part 173 is arranged between the second anti-falling part 172 and the bottom of the crucible furnace 1, the elastic compression part 173 is sleeved on the ejector rod 17, and two ends of the elastic compression part 173 are respectively abutted against the bottom of the crucible furnace 1 and the surface of the second anti. Preferably, the second anti-slip member 172 is a nut screwed to the ram 17, it being understood that the outer diameter of the nut is larger than the diameter of the second through hole 16, the elastic compression member 173 is a ring spring, and the inner diameter of the ring spring is smaller than the outer diameter of the nut so that the ring spring is caught between the nut and the bottom of the crucible furnace.
Referring to fig. 1 and 3, a notch 15 is arranged at the edge of the upper end of the crucible furnace 1, and the notch 15 is used for matching and connecting with an X-ray diffractometer.
Referring to fig. 4 and 5, when the sodium metaborate is measured by using the sample stage for measuring a liquid sample and the X-ray diffractometer in the X-ray diffractometer according to the embodiment, it can be seen from the figures that when the sodium metaborate is measured by using the sample stage in the embodiment, the bond length between atoms is slightly increased due to the high temperature, and a better result can be obtained.
According to the sample stage for measuring the liquid sample for the X-ray diffractometer, the temperature control thermocouple inserted into the crucible furnace controls the temperature of the crucible furnace, so that a quartz crucible arranged in the crucible furnace is heated and controlled, the problem that a water bath kettle needs to be filled with water to heat when the liquid is measured by the existing diffractometer is solved, and meanwhile, the heating range of the heating stage is widened due to the fact that a hearth has higher adjustable temperature; the position of the sample table is adjusted through the adjusting assembly and the horizontal adjusting mechanism, the overall height of the sample table is adjusted through the lifting mechanism, and the whole sample table is compact in structure and convenient to operate; simultaneously, the bottom of the furnace body is provided with an ejector rod capable of freely moving up and down, so that the crucible can be conveniently taken and placed, the sample platform does not need to be replaced during testing, the crucible in the crucible furnace only needs to be taken out, and the sample can be replaced, and the operation is simple and convenient.
The foregoing is merely a detailed description of the present application, and it should be noted that modifications and embellishments could be made by those skilled in the art without departing from the principle of the present application, and these should also be considered as the protection scope of the present application.
Claims (6)
1. A sample stage for measuring a liquid sample for an X-ray diffractometer, comprising: the temperature-adjustable crucible furnace comprises a crucible furnace (1) with adjustable temperature, a quartz crucible (2) used for containing a sample and a temperature-control thermocouple (3), wherein a groove (14) is formed in the upper surface of the crucible furnace (1) in an inwards concave mode, the quartz crucible (2) is arranged in the groove (14), and the temperature-control thermocouple (3) is inserted into the crucible furnace (1) to adjust the temperature of the crucible furnace (1);
the crucible furnace comprises a crucible furnace body (1), a furnace fixing seat (4) arranged at the bottom of the crucible furnace body (1), a first supporting column (5) and a level gauge (6) which are respectively arranged on the upper surface of the furnace fixing seat (4), an adjusting component (7) arranged on the lower surface of the furnace fixing seat (4) and a supporting device (8) connected with the adjusting component (7) to support the adjusting component (7), wherein a plurality of first supporting columns (5) are arranged and are connected with the bottom of the crucible furnace body (1) to support the crucible furnace body (1), the level gauge (6) is used for measuring the inclination angle of a sample table, and the adjusting component (7) is used for adjusting the inclination angle of the sample table;
the supporting device (8) comprises a lifting mechanism (81) with adjustable height and a horizontal adjusting mechanism (82) which is arranged on the lifting mechanism (81) and can adjust the horizontal position, a second supporting column (83) is arranged on the surface, away from the lifting mechanism (81), of the horizontal adjusting mechanism (82), and the top end of the second supporting column (83) is connected with the adjusting component (7);
elevating system (81) include bottom plate (811), liftable cut fork mechanism (812) and control cut first regulation pole (813) that fork mechanism (812) goes up and down, cut fork mechanism (812) and be equipped with two pairs from top to bottom, wherein locate the lower extreme cut fork mechanism (812) and arrange in on bottom plate (811), just the horizontal one side of the bottom of cutting fork mechanism (812) with bottom plate (811) fixed connection, two pairs cut fork mechanism (812) and articulate from top to bottom, and articulated department transverse connection has first horizontal pole (812-1) and second horizontal pole (812-2), first regulation pole (813) are rotatable to pass first horizontal pole (812-1) and second horizontal pole (812-2) in proper order and to stretch out second horizontal pole (812-2), first regulation pole (813) and first horizontal pole (812-1) threaded connection, first regulation pole (813) stretch out the one end of second horizontal pole (812-2) is equipped with and prevents that the institute from The first adjusting rod (813) is separated from the first anti-separation piece (814) of the second cross rod (812-2);
the base plate (811) and the horizontal adjusting mechanism (82) are connected with at least two diagonally arranged telescopic rods (815), the horizontal adjusting mechanism (82) comprises a fixed seat (822) relatively fixed to the top end of the telescopic rod (815), a sliding table (823) arranged on the fixed seat (822) and capable of horizontally sliding relative to the fixed seat (822), and a second adjusting rod (824) driving the sliding table (823) to slide relative to the fixed seat (822), and the second supporting column (83) is arranged on the upper surface of the sliding table (823).
2. The sample stage for measuring a liquid sample according to claim 1, wherein: a notch (15) is arranged at the edge of the upper end of the crucible furnace (1), and the notch (15) is used for being connected with an X-ray diffractometer in a matching mode.
3. The sample stage for measuring a liquid sample according to claim 2, wherein: the hearth (12) of the crucible furnace (1) is made of zirconia polycrystal fiber materials.
4. The sample stage for measuring a liquid sample according to claim 1, wherein: the adjusting component (7) comprises a supporting platform (71) connected with the second supporting column (83) and three supporting adjusting feet (72) uniformly arranged on the supporting platform (71).
5. The sample stage for measuring a liquid sample according to claim 1, wherein: the crucible furnace (1) is provided with a second through hole (16) coaxial with the groove (14), a push rod (17) penetrates through the second through hole (16), and the push rod (17) is used for pushing the quartz crucible (2) arranged in the groove (14) upwards.
6. The sample stage for measuring a liquid sample according to claim 5, wherein: a quartz backing plate (18) used for supporting the quartz crucible (2) is arranged at the bottom of the groove (14), one end of the mandril (17) passes through the second through hole (16) and is contacted with the quartz backing plate (18), a convex shoulder (171) for preventing the ejector rod (17) from falling is arranged at the contact part of the ejector rod (17) and the quartz backing plate (18), the other end of the ejector rod (17) extends out of the second through hole (16), the extending end of the ejector rod (17) is provided with a second anti-falling part (172) for preventing the ejector rod (17) from falling off upwards, an elastic compression piece (173) is arranged between the second anti-falling piece (172) and the bottom of the crucible furnace (1), the elastic compression piece (173) is sleeved on the ejector rod (17) and two ends of the elastic compression piece (173) are respectively abutted against the bottom of the crucible furnace (1) and the surface of the second anti-falling piece (172).
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 |
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| CN107966463A CN107966463A (en) | 2018-04-27 |
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| 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 |
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| JP3697246B2 (en) * | 2003-03-26 | 2005-09-21 | 株式会社リガク | X-ray diffractometer |
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