CN110161439A - A kind of heating device of HIGH-TEMPERATURE NMR PROBE and its application - Google Patents
A kind of heating device of HIGH-TEMPERATURE NMR PROBE and its application Download PDFInfo
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- CN110161439A CN110161439A CN201910416834.3A CN201910416834A CN110161439A CN 110161439 A CN110161439 A CN 110161439A CN 201910416834 A CN201910416834 A CN 201910416834A CN 110161439 A CN110161439 A CN 110161439A
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- resistive heater
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
- G01R33/00—Arrangements or instruments for measuring magnetic variables
- G01R33/20—Arrangements or instruments for measuring magnetic variables involving magnetic resonance
- G01R33/28—Details of apparatus provided for in groups G01R33/44 - G01R33/64
- G01R33/32—Excitation or detection systems, e.g. using radio frequency signals
- G01R33/34—Constructional details, e.g. resonators, specially adapted to MR
- G01R33/34015—Temperature-controlled RF coils
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- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
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Abstract
The invention belongs to high temperature nuclear magnetic resonance technical field of heating, and specifically disclose heating device and its application of a kind of HIGH-TEMPERATURE NMR PROBE, it includes more ceramic tubes and two resistive heaters, more ceramic tubes circumferentially arrange, and along the through hole of ceramic tube length direction distribution there are four being opened up in every ceramic tube, two of them through hole is located at the inside of circumference, another two through hole is located at the outside of circumference, and all through holes that adjacent ceramic pipe is located inside circumference are located on the first circumference, all through holes that adjacent ceramic pipe is located at periphery are located on the second circumference；A piece resistive heater sequentially passes through each through hole on the first circumference, and another resistive heater sequentially passes through each through hole on the second circumference, be passed through contrary electric current in two resistive heaters.The magnetic field that the present invention can be such that resistance wire generates is cancelled out each other, and the additional field that electric current generates is eliminated, and is had the advantages that structure is simple, is operated conveniently.
Description
Technical field
The invention belongs to high temperature nuclear magnetic resonance technical field of heating, more particularly, to a kind of HIGH-TEMPERATURE NMR PROBE
Heating device and its application.
Background technique
High temperature nuclear magnetic resonance is the technology for realizing nuclear magnetic resonance at high temperature, the structure of technology substance under researching high-temperature
Develop and is had important application with the chemical reaction under high temperature.The heating structure and heating method of HIGH-TEMPERATURE NMR PROBE at present
To sequentially pass through resistive heater all the way in the diplopore circumferentially arranged ceramics, heated using the Joule effect of electric current, such as Fig. 1
It is shown.
The advantages of existing this heating method be the resistance wire current direction wound back and forth on the contrary, can perpendicular to
Changes of magnetic field caused by cancellation current on the direction (i.e. horizontal direction) of ceramic tube.But this method is above and below diplopore ceramics
The curved place of both ends resistance wire, sense of current is identical, can generate additional magnetic field again, to being parallel to ceramic tube direction
The magnetic field of (i.e. vertical direction) impacts so that the obtained experiment value of measurement occur with the size of electric current it is different degrees of inclined
It moves.Although the method that can be then averaged by acquiring the experiment value of two current directions eliminates this offset,
Acquisition extends acquisition time twice, reduces conventional efficient.
Therefore, aiming at the problem that measurement result caused by the heating method of existing HIGH-TEMPERATURE NMR PROBE deviates, have
Necessity is studied and is designed to obtain a kind of new HIGH-TEMPERATURE NMR PROBE heating structure and heating method.
Summary of the invention
Aiming at the above defects or improvement requirements of the prior art, adding the present invention provides a kind of HIGH-TEMPERATURE NMR PROBE
Thermal and its application pass through the ceramics of circumferential arrangement by two-way resistance wire to form inside and outside heating coil, and two-way electricity
The current direction of silk is hindered on the contrary, eliminating the additional magnetic that heated current generates to which the magnetic field energy for generating resistance wire is cancelled out each other
, have the advantages that structure simply, operate conveniently, when heating element as HIGH-TEMPERATURE NMR PROBE, core can be effectively improved
The accuracy of magnetic detection.
To achieve the above object, according to one aspect of the present invention, a kind of heating of HIGH-TEMPERATURE NMR PROBE is proposed
Device comprising more ceramic tubes and two resistive heaters, wherein more ceramic tubes circumferentially arrange, and every ceramic tube
It inside opening up there are four the through hole along the distribution of ceramic tube length direction, two of them through hole is located at the inside of circumference, and another two
A through hole is located at the outside of circumference, and adjacent ceramic pipe is located at all through holes of inside circumference and is located on the first circumference,
All through holes that adjacent ceramic pipe is located at periphery are located on the second circumference；A piece resistive heater sequentially passes through
For each through hole on one circumference to form heating inner ring, another resistive heater sequentially passes through respectively passing through on the second circumference
Through-hole is to form heating outer ring, in use, contrary electric current is passed through in two resistive heaters, so that adjacent ceramic pipe
The current direction of interior resistive heater on the contrary, and two resistive heaters at same ceramic tube both ends current direction also phase
Instead.
As it is further preferred that the ceramic tube is using high temperature resistant and nonconducting ceramics are made at high temperature.
As it is further preferred that the resistive heater is made of dystectic no magnetic metal material.
As it is further preferred that the diameter of the resistive heater is preferably 0.4mm~0.6mm, further preferably
0.5mm。
As it is further preferred that the diameter of the ceramic tube is preferably 3.0mm-4.5mm, further preferably 3.5mm.
As it is further preferred that the diameter of the through hole is preferably 0.05mm bigger than the diameter of resistive heater, and it is each
The center of through hole is preferably designed for a quarter of ceramic pipe diameter away from the distance of ceramic tube hub.
It is another aspect of this invention to provide that providing a kind of heating device answering in HIGH-TEMPERATURE NMR PROBE
With.
In general, through the invention it is contemplated above technical scheme is compared with the prior art, mainly have below
Technological merit:
1. two-way resistance wire is passed through four hole ceramics of circumferential arrangement to form heating layer, and two-way resistance wire by the present invention
Current direction on the contrary, make ceramic tube both ends resistive heater knee both forward and reverse directions electric current generate both forward and reverse directions magnetic field
Also the problem of capable of cancelling out each other, efficiently solving the additional field for being parallel to ceramic tube direction due to caused by electric current all the way.
2. the present invention also the dimensional parameters of key component are studied and have been designed, it is determined that resistive heater it is best
Size guarantees to add heat availability and stability, it is determined that the optimum size of ceramic tube guarantees to protect in the case where ceramic tube intensity
Heating efficiency is demonstrate,proved, the dimensional parameters for additionally combining resistive heater and ceramic tube have determined the optimum size of through hole, with
Guarantee effective uniformity assembled and heat of resistive heater.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of existing heating device；
Fig. 2 is the structural schematic diagram of heating device provided in an embodiment of the present invention；
Fig. 3 is the structural schematic diagram of ceramic tube provided in an embodiment of the present invention；
Fig. 4 is the schematic diagram of current direction in heating device provided in an embodiment of the present invention；
Fig. 5 is application exemplary diagram of the heating device provided in an embodiment of the present invention in HIGH-TEMPERATURE NMR PROBE.
In all the appended drawings, identical appended drawing reference is used to denote the same element or structure, in which:
1- ceramic tube, 2- resistive heater, 3- through hole, 4- metal screen layer, 5- resonance coil, 6- thermal insulation layer, 7- are cold
But layer, 8- heating chamber, 9- temperature measuring element.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.As long as in addition, technical characteristic involved in the various embodiments of the present invention described below
Not constituting a conflict with each other can be combined with each other.
As shown in Fig. 2, a kind of heating device of HIGH-TEMPERATURE NMR PROBE provided in an embodiment of the present invention comprising more
Ceramic tube 1 and two resistive heaters 2, wherein more ceramic tubes 1 circumferentially arrange, i.e., every ceramic tube 1 is arranged vertically, that
This is adjacent and fits closely, to surround an annular shape.As shown in figure 3, opening up in every ceramic tube 1, there are four along ceramic tube 1
The through hole 3 of length direction distribution, as shown in Fig. 2, two through holes 3 in same root ceramic tube 1 are located at circumference (annular shape)
Inside, the two through holes are defined as the first through hole and the second through hole, and another two through hole 3 is located at circumference (annular shape)
Outside, the two through holes are defined as third through hole and the 4th through hole, and adjacent ceramic pipe 1 is located at all of inside circumference
Through hole is located on the first circumference, and all through holes that adjacent ceramic pipe 1 is located at periphery are located on the second circumference；One adds
Hot water radiation wire 2 (being defined as the first resistive heater) sequentially passes through each through hole on the first circumference to form heating inner ring, example
If mode that is first up and then down or getting on, get off sequentially passes through each through hole, another resistive heater 2 (is defined as the second heating electricity
Resistance silk) each through hole on the second circumference is sequentially passed through to form heating outer ring, mode is installed with the first resistive heater
Unanimously, resistive heater 2 sequentially passes through serpentine-like distribution after each through hole.Electric current in two resistive heaters 2 on the contrary, with
This make the current direction of the resistive heater 2 in adjacent ceramic pipe 1 on the contrary, and 1 both ends of same ceramic tube two heating electricity
The current direction for hindering silk 2 is also opposite.
Specifically, for example shared N root ceramic tube 1, is successively defined as the first ceramic tube to N ceramic tube, then first
Resistive heater penetrates lower section above the first through hole of the first ceramic tube and is pierced by, then penetrates through from the second of the first ceramic tube
Top is penetrated below hole to be pierced by, then is penetrated lower section above the first through hole of the second ceramic tube and be pierced by, then make pottery from second
Top is penetrated below second through hole of porcelain tube to be pierced by, then is penetrated lower section above the first through hole of third ceramic tube and worn
Out, then below the second through hole of third ceramic tube top is penetrated to be pierced by, and so on, then from the first of N ceramic tube
Lower section is penetrated above through hole to be pierced by, and top is finally penetrated below the second through hole of N ceramic tube and is pierced by.Similarly,
Second resistive heater penetrates lower section above the third through hole of the first ceramic tube and is pierced by, then from the 4th of the first ceramic tube
Top is penetrated below through hole to be pierced by, then penetrates above the third through hole of the second ceramic tube lower section and is pierced by, then from the
Top is penetrated below 4th through hole of two ceramic tubes to be pierced by, then is penetrated down above the third through hole of third ceramic tube
Side is pierced by, then is penetrated below the 4th through hole of third ceramic tube top and be pierced by, and so on, then from N ceramic tube
Lower section is penetrated above third through hole to be pierced by, and top is finally penetrated below the 4th through hole of N ceramic tube and is pierced by.
Since same root ceramic tube is set on the same circumference there are two through hole, resistive heater is penetrated by a through hole
(such as from bottom to up) is pierced by (then from top to bottom) by another through hole, then penetrates passing through for (then from bottom to up) adjacent ceramic pipe
In through-hole, as shown in figure 4, so that being located at the resistive heater in two through holes on same circumference in same root ceramic tube
Current direction on the contrary, the current direction of the resistive heater in two through hole of adjacent ceramic pipe on the contrary, and due to same ceramics
Two resistive heaters are equipped in pipe, and the current direction of two resistive heaters is on the contrary, make at same root ceramic tube upper end
The current direction in (i.e. resistive heater knee) on the contrary, at same root ceramic tube lower end (i.e. resistive heater knee) electricity
Stream direction is also on the contrary, will not generate volume to cancel out each other from there through the magnetic field that the electric current of both forward and reverse directions generates both forward and reverse directions
Outer magnetic field.
Specifically, dystectic no magnetic metal such as molybdenum, tungsten, tantalum, niobium etc. can be used in resistive heater.The material of ceramic tube can
To be the high temperature resistants such as aluminium oxide ceramics and nonconducting ceramics at high temperature.Further, two resistive heaters connect direction
Opposite direct current, to generate contrary electric current.
It is found in practical application, electric current is big when resistive heater is too thin is easy to blow, and resistive heater slightly then heats very much
Very big electric current is needed to high temperature, so on the one hand than relatively hazardous, there are security risks, on the other hand to the DC power supply of pressure stabilizing
Have damage, by it is continuous the study found that resistive heater 2 diameter design be 0.4mm~0.6mm, be preferably designed for
0.5mm, can achieve preferable heating effect, and the service life of resistance wire is longer.In order to guarantee that resistive heater 2 is effectively worn
It crosses, is the diameter+0.05mm of resistive heater by the diameter design of through hole.
Further, when design, the specific size phase of the height and application HIGH-TEMPERATURE NMR PROBE of ceramic tube 1
It closes, is designed as needed, for example, 40mm.In order to guarantee heating effect and ceramic tube intensity, the present invention is comprehensive to be added
The dimensional parameters of hot water radiation wire and through hole have carried out researching and designing to the dimensional parameters of ceramic tube, specifically, by ceramic tube 1
Diameter design is 3.0-4.5mm, is further preferably designed as 3.5mm, so avoids ceramic pipe diameter is too small from causing to open up perforation
Hole rear wall is relatively thin, the problem for causing the inadequate easy fracture of intensity broken, while avoiding diameter excessive so that heating device overall alignment
Ceramic tube it is less, and then cause resistive heater total length shorter, the low problem of heating efficiency.In addition, the center of through hole 3
Distance away from ceramic tube central axis is preferably designed for a quarter of ceramic pipe diameter, to guarantee the uniformity of heating.
Heating device of the invention can be applicable in HIGH-TEMPERATURE NMR PROBE, as shown in figure 5, heating of the invention is filled
I heating element as HIGH-TEMPERATURE NMR PROBE is set, which includes metal screen layer 4, resonance coil 5
With thermal insulation layer 6 and cooling layer 7, metal screen layer 4 is the cavity body structure of upper end closed lower ending opening, and thermal insulation layer 6 is wrapped in metal
Outside shielded layer 4, and the inside of the metal screen layer 4 of the bottom of thermal insulation layer 6 and cavity body structure forms heating chamber 8, cooling
Layer 7 is wrapped in the outside of entire thermal insulation layer 6, and for realizing the cooling of HIGH-TEMPERATURE NMR PROBE, heating device I of the invention is set
Between metal screen layer 4 and thermal insulation layer 6, the upper end of resonance coil 5 is placed in the inside of heating chamber 8, lower end sequentially pass through every
Thermosphere 6 and cooling layer 7, are then connected with resonant circuit, in addition, HIGH-TEMPERATURE NMR PROBE further includes being inserted into thermal insulation layer from outside
Temperature measuring element 9 in 6, such as thermocouple, realize the measurement of temperature.In use, two resistive heaters of the invention are respectively and directly
Galvanic electricity source is connected and makes current direction on the contrary, when HIGH-TEMPERATURE NMR PROBE work, carries out temperature measurement by temperature measuring element, so
The output electric current for the temperature control DC power supply that the temperature controller connecting afterwards with temperature measuring element is measured according to temperature measuring element, electric current is by heating
Resistance wire generates heat, and the sample being located in resonance coil is made to reach required temperature.
Compared with previous Resistant heating mode, the method that the present invention uses two-way resistance wire, and two-way resistance wire
Current direction make the magnetic field generated at ceramic tube both ends by electric current that can also cancel out each other on the contrary, effectively eliminate heating electricity
The raw additional field contribution of miscarriage, helps to obtain accurate nuclear magnetic resonance data at high temperature.Relative to using single channel resistance
Silk, by changing current direction, acquisition carrys out offset magnetic field variation twice and has an impact ground method to data, and The present invention reduces adopt
Collect the time.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to
The limitation present invention, any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should all include
Within protection scope of the present invention.
Claims (7)
1. a kind of heating device of HIGH-TEMPERATURE NMR PROBE, which is characterized in that including more ceramic tubes (1) and two heating electricity
It hinders silk (2), wherein more ceramic tubes (1) circumferentially arrange, and open up that there are four along ceramic tube (1) in every ceramic tube (1)
The through hole (3) of length direction distribution, two of them through hole (3) are located at the inside of circumference, and another two through hole (3) is located at circle
The outside in week, and adjacent ceramic pipe (1) is located at all through holes of inside circumference and is located on the first circumference, adjacent ceramic pipe
(1) it is located on the second circumference positioned at all through holes of periphery；A piece resistive heater (2) sequentially passes through the first circle
For each through hole on week to form heating inner ring, another resistive heater (2) sequentially passes through respectively passing through on the second circumference
Through-hole is to form heating outer ring, in use, contrary electric current is passed through in two resistive heaters (2), so that adjacent pottery
The current direction of resistive heater (2) in porcelain tube (1) on the contrary, and same ceramic tube (1) both ends two resistive heaters (2)
Current direction it is also opposite.
2. the heating device of HIGH-TEMPERATURE NMR PROBE as described in claim 1, which is characterized in that the ceramic tube (1) is adopted
Nonconducting ceramics are made with high temperature resistant and at high temperature.
3. the heating device of HIGH-TEMPERATURE NMR PROBE as described in claim 1, which is characterized in that the resistive heater
(2) it is made of dystectic no magnetic metal material.
4. the heating device of HIGH-TEMPERATURE NMR PROBE as described in claim 1, which is characterized in that the resistive heater
(2) diameter is preferably 0.4mm~0.6mm, further preferably 0.5mm.
5. the heating device of HIGH-TEMPERATURE NMR PROBE according to any one of claims 1-4, which is characterized in that the ceramics
The diameter for managing (1) is preferably 3.0mm-4.5mm, further preferably 3.5mm.
6. the heating device of HIGH-TEMPERATURE NMR PROBE as described in any one in claim 1-5, which is characterized in that the perforation
The diameter in hole (3) is preferably 0.05mm bigger than the diameter of resistive heater, and the center of each through hole (3) is away from ceramic tube (1) center
Distance be preferably designed for a quarter of ceramic pipe diameter.
7. a kind of application of heating device as claimed in any one of claims 1 to 6 in HIGH-TEMPERATURE NMR PROBE.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910416834.3A CN110161439A (en) | 2019-05-20 | 2019-05-20 | A kind of heating device of HIGH-TEMPERATURE NMR PROBE and its application |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910416834.3A CN110161439A (en) | 2019-05-20 | 2019-05-20 | A kind of heating device of HIGH-TEMPERATURE NMR PROBE and its application |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112055428A (en) * | 2020-07-28 | 2020-12-08 | 中国原子能科学研究院 | Reciprocating heating coil structure for realizing high-temperature environment in vacuum |
| CN113009389A (en) * | 2019-12-19 | 2021-06-22 | 中国科学院宁波材料技术与工程研究所 | Laser heating high-temperature nuclear magnetic resonance probe and device |
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| CN113009389B (en) * | 2019-12-19 | 2022-09-23 | 中国科学院宁波材料技术与工程研究所 | Laser heating high-temperature nuclear magnetic resonance probe and device |
| CN112055428A (en) * | 2020-07-28 | 2020-12-08 | 中国原子能科学研究院 | Reciprocating heating coil structure for realizing high-temperature environment in vacuum |
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Application publication date: 20190823 |