Detection device for measuring sample characteristics at low temperature by X-ray diffractometer
阅读说明：本技术 一种用于x射线衍射仪在低温下测量样品特性的检测装置 (Detection device for measuring sample characteristics at low temperature by X-ray diffractometer ) 是由 张所峰 刘川 王军龙 胡婷婷 于 2020-07-23 设计创作，主要内容包括：本发明公开一种用于X射线衍射仪在低温下测量样品特性的检测装置,包括控温加热片、低温样品架、绝缘隔热套、液氮输送管。控温加热片为铁镍合金材质且两端固定。低温样品架上镶嵌有温度传感器并紧贴控温加热片。绝缘隔热套紧靠低温样品架并由密封圈密封。液氮输送管装在绝缘隔热套上,为内、中、外三层结构。内层为液氮输入管,中间层为液氮输出管,外层为隔热保温管。冷却套为两个半圆形结构,中间有冷却通道。本发明采用液氮输送管输送液氮到控温加热片上来实现给样品降温的目的,并通过低温样品架与控温加热片之间的温度传感器反馈温度到控制软件来调节并控制样品温度,使样品温度始终稳定在设定温度。(The invention discloses a detection device for measuring sample characteristics of an X-ray diffractometer at low temperature. The temperature control heating plate is made of iron-nickel alloy and two ends of the temperature control heating plate are fixed. The low-temperature sample rack is embedded with a temperature sensor and is tightly attached to a temperature control heating sheet. The insulating and heat insulating sleeve is tightly close to the low-temperature sample rack and sealed by a sealing ring. The liquid nitrogen conveying pipe is arranged on the insulating heat-insulating sleeve and is of an inner layer structure, a middle layer structure and an outer layer structure. The inner layer is a liquid nitrogen input pipe, the middle layer is a liquid nitrogen output pipe, and the outer layer is a heat insulation pipe. The cooling jacket is in two semicircular structures, and a cooling channel is arranged in the middle of the cooling jacket. The invention adopts the liquid nitrogen delivery pipe to deliver liquid nitrogen to the temperature control heating sheet to realize the purpose of cooling the sample, and feeds back the temperature to the control software through the temperature sensor between the low-temperature sample rack and the temperature control heating sheet to adjust and control the temperature of the sample, so that the temperature of the sample is always stabilized at the set temperature.)
1. A detecting device for measuring characteristics of a sample at a low temperature by an X-ray diffractometer, characterized in that: including low temperature sample frame, accuse temperature heating plate and liquid nitrogen conveyer pipe, sealed the fixing on the chassis be provided with on the low temperature sample frame accuse temperature heating plate is used for doing accuse temperature heating plate on the low temperature sample frame provides liquid nitrogen cooling be provided with liquid nitrogen input tube, the liquid nitrogen that communicates in order in the liquid nitrogen conveyer pipe and collect pipe and liquid nitrogen output tube.
2. The detecting unit for measuring the characteristics of the sample at a low temperature by the X-ray diffractometer according to claim 1, wherein: the temperature control heating plate is made of an iron-nickel alloy material; two ends of a temperature control heating sheet for placing a sample and controlling the temperature of the sample are tightly pressed on the fixing columns on the base plate, and the middle part of the temperature control heating sheet is positioned on the low-temperature sample rack.
3. The detecting unit for measuring the characteristics of the sample at a low temperature by the X-ray diffractometer according to claim 1, wherein: the low-temperature sample frame is fixed on the chassis in a sealing mode through a sealing ring I, and the temperature sensor is embedded in the red copper plate on the low-temperature sample frame and is tightly attached to the temperature control heating sheet.
4. The detecting unit for measuring the characteristics of the sample at a low temperature by the X-ray diffractometer according to claim 1, wherein: the inner layer of the liquid nitrogen conveying pipe is the liquid nitrogen input pipe, and the liquid nitrogen input pipe is a stainless steel pipe with a connecting flange; one end of the liquid nitrogen input pipe extends into the low-temperature sample rack, and the other end of the liquid nitrogen input pipe is welded with the liquid nitrogen insertion pipe and inserted into the liquid nitrogen storage device.
5. The detecting unit for measuring the characteristics of the sample at a low temperature by the X-ray diffractometer according to claim 1, wherein: the middle layer of the liquid nitrogen conveying pipe is the liquid nitrogen output pipe, one end of the liquid nitrogen collecting pipe extends into the low-temperature sample frame and is sleeved outside the liquid nitrogen input pipe to be concentric with the liquid nitrogen input pipe, the other end of the liquid nitrogen collecting pipe is welded to the top of the liquid nitrogen output pipe through a connecting flange on the liquid nitrogen input pipe, and the liquid nitrogen collecting pipe is communicated with the liquid nitrogen output pipe; and the tail end of the liquid nitrogen output pipe is welded to the liquid nitrogen extraction joint.
6. The detecting unit for measuring the characteristics of the sample at a low temperature by the X-ray diffractometer according to claim 1, wherein: the outer layer of the liquid nitrogen conveying pipe is a heat insulation pipe, the heat insulation pipe is a whole stainless steel corrugated pipe, the heat insulation pipe is sleeved outside the liquid nitrogen output pipe, one end of the heat insulation pipe is welded on a connecting flange on the liquid nitrogen input pipe, and the other end of the heat insulation pipe is welded with the vacuum connecting joint.
7. The detecting unit for measuring the characteristics of the sample at a low temperature by the X-ray diffractometer according to claim 1, wherein: the outside cladding that the pipe was collected to liquid nitrogen has insulating heat insulating sleeve, insulating heat insulating sleeve is made by polytetrafluoroethylene material, and sealing washer two sealing connection are passed through to insulating heat insulating sleeve's one end on the low temperature sample frame, the other end is fixed through sealing washer three flange department on the liquid nitrogen input tube.
8. The detecting unit for measuring the characteristics of the sample at a low temperature by the X-ray diffractometer according to claim 1, wherein: a cooling jacket is arranged at a connecting flange on the liquid nitrogen input pipe, and a cooling water inlet pipe and a cooling water outlet pipe in the cooling jacket are connected to a cooling system of the X-ray diffractometer; and cooling water enters the cooling jacket through the cooling water inlet pipe, firstly enters the cooling jacket at the other end through the cooling channel through the connecting water pipe, and then returns to the cooling system of the X-ray diffractometer through the cooling channel through the cooling water outlet pipe.
Technical Field
The invention relates to the technical field of low-temperature detection devices, in particular to a detection device for measuring sample characteristics at low temperature by an X-ray diffractometer.
Background
The X-ray diffractometer takes a Bragg experimental device as a prototype, integrates the achievements of mechanical and electronic technologies and the like, and is a diffraction experimental device which irradiates a polycrystalline sample with characteristic X-rays and records diffraction information with a radiation detector. The X-ray diffractometer can analyze the structure and composition of a substance, and can accurately measure the structure of a molecule without destroying a sample. X-ray diffraction methods are ideally very efficient for studying materials of structures, and provide a number of essential data for liquids and amorphous solids. X-ray diffraction is considered to be the most effective tool.
The conventional X-ray diffractometer can only detect a sample in normal-temperature air when testing the sample, can only measure the structure and the composition of molecules of the sample at normal temperature, cannot measure the crystal structure change of the sample or the crystallinity change of various substances at low temperature, and needs a detection device capable of detecting the crystal sample at low temperature.
Disclosure of Invention
The invention provides a detection device for an X-ray diffractometer to measure sample characteristics at low temperature, aiming at the problem that the crystal structure change of a sample or the crystallinity change of various substances at low temperature cannot be measured.
In order to achieve the purpose, the invention provides the following scheme: the invention provides a detection device for measuring sample characteristics of an X-ray diffractometer at low temperature, which comprises a low-temperature sample frame, a temperature control heating sheet and a liquid nitrogen delivery pipe, wherein the low-temperature sample frame hermetically fixed on a chassis is provided with the temperature control heating sheet, and the liquid nitrogen delivery pipe for providing liquid nitrogen cooling for the temperature control heating sheet on the low-temperature sample frame is internally provided with a liquid nitrogen input pipe, a liquid nitrogen receiving pipe and a liquid nitrogen output pipe which are sequentially communicated.
Preferably, the temperature control heating plate is made of an iron-nickel alloy material; two ends of a temperature control heating sheet for placing a sample and controlling the temperature of the sample are tightly pressed on the fixing columns on the base plate, and the middle part of the temperature control heating sheet is positioned on the low-temperature sample rack.
Preferably, the low-temperature sample frame is fixed on the chassis in a sealing mode through a sealing ring I, and the temperature sensor is embedded in the red copper plate on the low-temperature sample frame and is tightly attached to the temperature control heating sheet.
Preferably, the inner layer of the liquid nitrogen conveying pipe is the liquid nitrogen input pipe, and the liquid nitrogen input pipe is a stainless steel pipe with a connecting flange; one end of the liquid nitrogen input pipe extends into the low-temperature sample rack, and the other end of the liquid nitrogen input pipe is welded with the liquid nitrogen insertion pipe and inserted into the liquid nitrogen storage device.
Preferably, the middle layer of the liquid nitrogen conveying pipe is the liquid nitrogen output pipe, one end of the liquid nitrogen collecting pipe extends into the low-temperature sample rack and is sleeved outside the liquid nitrogen input pipe to be concentric with the liquid nitrogen input pipe, the other end of the liquid nitrogen collecting pipe is welded to the top of the liquid nitrogen output pipe through a connecting flange on the liquid nitrogen input pipe, and the liquid nitrogen collecting pipe is communicated with the liquid nitrogen output pipe; and the tail end of the liquid nitrogen output pipe is welded to the liquid nitrogen extraction joint.
Preferably, the outer layer of the liquid nitrogen conveying pipe is a heat insulation pipe, the heat insulation pipe is a whole stainless steel corrugated pipe, the heat insulation pipe is sleeved outside the liquid nitrogen output pipe, low-temperature-resistant heat insulation materials are coated between the heat insulation pipe and the liquid nitrogen output pipe, one end of the heat insulation pipe is welded on a connecting flange on the liquid nitrogen input pipe, and the other end of the heat insulation pipe is welded with the vacuum connecting joint.
Preferably, the liquid nitrogen collecting pipe is externally coated with an insulating heat-insulating sleeve, the insulating heat-insulating sleeve is made of polytetrafluoroethylene materials, one end of the insulating heat-insulating sleeve is hermetically connected to the low-temperature sample rack through a second sealing ring, and the other end of the insulating heat-insulating sleeve is fixed to a connecting flange on the liquid nitrogen input pipe through a third sealing ring.
Preferably, a cooling jacket is arranged at a connecting flange on the liquid nitrogen input pipe, and a cooling water inlet pipe and a cooling water outlet pipe in the cooling jacket are connected to a cooling system of the X-ray diffractometer; and cooling water enters the cooling jacket through the cooling water inlet pipe, firstly enters the cooling jacket at the other end through the cooling channel through the connecting water pipe, and then returns to the cooling system of the X-ray diffractometer through the cooling channel through the cooling water outlet pipe.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention adopts the liquid nitrogen delivery pipe to extract the liquid nitrogen from the liquid nitrogen storage device to the low-temperature sample rack and controls the temperature of the low-temperature sample rack by the temperature control heating sheet to realize the purpose of controlling the temperature of the sample. The temperature is fed back to the control software through the temperature sensor on the low-temperature sample rack to adjust and control the temperature of the sample, so that the temperature of the sample is always stabilized at the set temperature.
The temperature control heating plate is made of iron-nickel alloy, and two ends of the temperature control heating plate are tightly pressed and fixed.
The low-temperature sample rack is in a hollow cylinder shape, and the top end of the low-temperature sample rack is embedded with a red copper plate and is tightly attached to the temperature control heating sheet. The bottom of the vacuum chamber is sealed by a sealing ring to meet the vacuum requirement.
The temperature sensor is embedded in the red copper plate on the low-temperature sample rack and is tightly attached to the temperature control heating sheet.
According to the invention, the insulating heat-insulating sleeve made of polytetrafluoroethylene material is arranged at the bottom of the low-temperature sample holder and is sealed by the sealing ring, so that liquid nitrogen leakage is prevented, and the personal safety of operators is protected.
The liquid nitrogen conveying pipe is arranged on the insulating heat-insulating sleeve and is sealed by the sealing ring. Liquid nitrogen leakage is prevented, and personal safety of operators is protected. The liquid nitrogen delivery pipe is of an inner layer structure, a middle layer structure and an outer layer structure. The inner layer is a liquid nitrogen input pipe, the middle layer is a liquid nitrogen output pipe, and the outer layer is a heat insulation pipe.
The cooling sleeve is sleeved at the joint of the liquid nitrogen conveying pipe and the insulating heat insulation sleeve and is of two semicircular structures with cooling channels in the middle. The cooling jacket is provided with a water inlet and outlet joint.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a schematic view of the water connections of the cooling jacket.
The device comprises a
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a detection device for an X-ray diffractometer to measure sample characteristics at low temperature, aiming at the problem that the crystal structure change of a sample or the crystallinity change of various substances at low temperature cannot be measured.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
As shown in fig. 1-2, the present embodiment provides a detection apparatus for measuring sample characteristics at low temperature by an X-ray diffractometer, which includes a temperature-controlled
Specifically, as shown in fig. 1, two ends of a temperature-controlled
Further, the inner layer of the liquid nitrogen conveying pipe is a liquid
During operation, liquid nitrogen is pumped into the liquid
As shown in figure 2, a
The invention adopts a liquid nitrogen conveying pipe to convey liquid nitrogen to the temperature
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein, and any reference signs in the claims are not intended to be construed as limiting the claim concerned.
The principle and the implementation mode of the invention are explained by applying a specific example, and the description of the embodiment is only used for helping to understand the method and the core idea of the invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In view of the above, the present disclosure should not be construed as limiting the invention.