CN208043721U - The crucible that crucible bottom is stepped - Google Patents

The crucible that crucible bottom is stepped Download PDF

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Publication number
CN208043721U
CN208043721U CN201820369918.7U CN201820369918U CN208043721U CN 208043721 U CN208043721 U CN 208043721U CN 201820369918 U CN201820369918 U CN 201820369918U CN 208043721 U CN208043721 U CN 208043721U
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China
Prior art keywords
crucible
sidewall
sample
stepped
crucible bottom
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CN201820369918.7U
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Chinese (zh)
Inventor
赵岩
陈刚
祁国恕
侯海盟
曾乐
裴江涛
范群
臧雪莉
张广鑫
李述贤
蒋帅
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Shenyang Academy Environmental Sciences
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Shenyang Academy Environmental Sciences
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Abstract

The utility model is related to a kind of crucible that crucible bottom is stepped, being that during the heat analysis of burning/gasification reaction of solid powdery sample, mass transfer condition is bad between sample and reaction gas is solved the problems, such as.The main points of the utility model are:It is made of sidewall of crucible and crucible bottom, it is characterised in that:Sidewall of crucible is cylindrical in hollow bevel, and crucible bottom inner face is stepped, and the arcuate midway point and sidewall of crucible minimum point of minimum step are to just.Sample is evenly laid out on the inner face of the crucible bottom, the minimum point and peak of sidewall of crucible face the reaction gas from horizontal direction, and minimum point is preceding, reaction gas directly reaches sample layer by forcing to transport, and the gas-phase product that simultaneous reactions generate quickly escapes by the pressure of reaction gas transports.

Description

The crucible that crucible bottom is stepped
Technical field
The utility model is related to heat analysis crucibles, and such crucible of application to carry out the burning of solid powdery sample, gas The method for changing response characteristic test, belongs to thermoanalysis technology field.
Background technology
Heat analysis is measured between the physical property of sample and temperature or time under the conditions of specified atmosphere and temperature programmed control A kind of analysis of modernization measuring technology of relationship includes mainly hot weight method (TG), derivative thermogravimetric amount method (DTG), differential scanning Calorimetry (DSC), poor (showing) heat analysis (DTA), thermo-mechanical analysis (TMA) and dynamic thermomechanical analysis (DMA) etc..Currently, hot Analytical technology has obtained in fields such as the energy, environment, physics, chemistry, chemical industry, metallurgy, geology, building materials, light textile, food, biologies To being widely applied, especially in energy and environment field, TG, DTG, DTA and DSC have become test and analysis sample Burning/gasification reaction characteristic and instruct reactor in actual industrial system to characterize and evaluation fuel fundamental property The important tool of design and operation.These four thermoanalysis technologies are both needed to sample (most of is solid powdery) being placed in certain knot In structure and the crucible of material, then the crucible for containing sample is put into heating furnace chamber, be passed through later specific reaction gas and Start to test under the temperature condition of program control, finally obtains quality, weight loss rate, temperature or the input thermal power and ginseng of sample Than object difference with test temperature or the change curve of time, to analyze burning/gasification reaction characteristic of sample.Currently, above-mentioned The structure of heating furnace chamber is divided into horizontal and two kinds rectilinear, wherein horizontal can not only ensure the measurement of sample quality not by The influence of its position, and heat buoyancy and the disturbance of the next quality signal of reaction gas turbulent zone can be made to minimize, thus obtain It is widely applied.For example, global famous precision instrument and Mettler Toledo Inc. of weighing apparatus manufacturer surmounts series TG/DSC thermal analyzers, with regard to all using horizontal heating furnace chamber.
In horizontal heating furnace chamber, reaction gas is imported by capillary near sample crucible, and with horizontal direction Initial velocity enters reaction compartment, when reaction gas is contacted with sample, that is, the change for chemically reacting and causing sample physical property occurs Change.However, at present institute widely used crucible be all made of have bottom surface hollow cylindrical structure, and crucible bottom surface it is interior, Outer surface is level.Sample tiles on the inner surface of bottom surface forms a horizontal sample layer, and crucible wall will be higher by sample Layer top is many, thus make it is horizontal come to reaction gas cannot rely on pressure and transport and directly reach sample layer, and need by Natural diffuseness act on, cross the obstruction of crucible wall, enter in crucible from the upper space of sample layer and contact with sample and instead It answers.Meanwhile the effusion for reacting the gas-phase product of generation also needs to realize by natural diffuseness.The above process causes expansion The increase for acting on contribution degree in overall reaction process control mechanism is dissipated, intrinsicization of the test data to make to sample The symbolical meanings for learning reactivity weaken, especially in the constant-temperature combustion of higher temperature/gasification reaction characteristic test, this influence It is more notable.
Invention content
In order to effectively reduce the influence of diffusion in solid powdery sample combustion, gasification reaction characteristic test, to Enhance symbolical meanings of the obtained data to the intrinsic chemical reaction characteristic of sample, the utility model provides a kind of crucible bottom The crucible being stepped.
What the purpose of this utility model was realized in:It is integrally formed by sidewall of crucible and crucible bottom group, it is characterised in that: Sidewall of crucible is cylindrical in hollow bevel, and it is in pipe angular cut to make mouth of pot, and crucible bottom inner face is stepped;Wherein lowest-order To just, height of the sidewall of crucible minimum point away from minimum cascaded surface is the minimum point of arcuate midway point and the sidewall of crucible, that is, pipe angular cut of ladder 0.5~1 mm;Height of the peak of sidewall of crucible away from highest cascaded surface is 1.5 ~ 2.5 mm;The height of every grade of ladder is 1-2 mm; The tangent value of angle is 1 between face and horizontal plane where pipe angular cut:3~1:1;The thickness of crucible bottom thinnest part and sidewall of crucible It is 0.5 mm;A diameter of 10 ~ 17 mm of crucible bottom outer surface.
The material of the utility model is high purity aluminium oxide or platinum.
Burning, the gasification reaction characteristic test of solid powdery sample are carried out using the crucible that above-mentioned crucible bottom is stepped Method be that sample is evenly laid out on all cascaded surfaces or other cascaded surfaces in addition to minimum ladder, sidewall of crucible it is minimum Point and peak face the reaction gas from horizontal direction, and minimum point, preceding, reaction gas transports direct arrival by forcing Sample layer, the gas-phase product that simultaneous reactions generate can also quickly escape by the pressure of reaction gas transports.
Compared with prior art, the utility model has the advantages that:
1, due in crucible sample layer in ladder be distributed, and mouth of pot be in pipe angular cut, the position where most of sample It sets and is higher than the sidewall of crucible i.e. minimum point of pipe angular cut, that is, be directly exposed in the reaction gas from horizontal direction, effectively reduce Contribution degree of the external diffusion in overall reaction process control mechanism before reaction.
2, the gas-phase product that reaction generates again may be by the pressure of reaction gas and transport and quickly escape, to reduce Contribution degree of the external diffusion in overall reaction process control mechanism after reaction.
Above-mentioned both sides advantageous effect means that influence of the diffusion to overall reaction process obtains in different links Weakening has been arrived, symbolical meanings of the obtained test data to the intrinsic chemical reactivity of sample are finally enhanced.
Description of the drawings
The utility model is described in further detail in the following with reference to the drawings and specific embodiments.
Fig. 1 is the sectional axonometric drawing of the utility model.
Fig. 2 is the A direction views of Fig. 1.
Specific implementation mode
Referring to Fig. 1 and 2, the crucible that crucible bottom is stepped is integrally formed by 3 groups of sidewall of crucible 2 and crucible bottom, and sidewall of crucible is in Hollow bevel is cylindrical, and it is in pipe angular cut to make mouth of pot, and crucible bottom inner face is in three-level stairstepping;Wherein minimum ladder is The arcuate midway point 33 of first order ladder 31 is with minimum 21 points of sidewall of crucible, that is, pipe angular cut to just, sidewall of crucible minimum point is away from first The height h1 of grade cascaded surface is 0.5 ~ 1 mm;Height h2 of the peak of sidewall of crucible away from highest cascaded surface, that is, third level cascaded surface be 1.5~2.5 mm;The height h3 of every grade of ladder is 1-2 mm;The tangent value of angle between pipe angular cut place face and horizontal plane It is 1:3~1:1;The thickness of crucible bottom thinnest part and sidewall of crucible is 0.5 mm;A diameter of the 10 ~ 17 of crucible bottom outer surface 32 mm。
The material of the utility model is high purity aluminium oxide or platinum.
The combustion gasification response characteristic that solid powdery sample is carried out using the crucible that above-mentioned crucible bottom is stepped is tested Method, it is specifically, the sample 1 of 5 ~ 9 mg is evenly laid out on all cascaded surfaces, also can only be laid on the second level and the third level On cascaded surface.The minimum point and peak of sidewall of crucible face the reaction gas from horizontal direction, and minimum point is preceding.According to pre- If heating and gas changeover program start to test, wherein the flow control of reaction gas is in 30 ~ 80 mLmin-1Range.Instead Should gas by force transport directly reach sample layer, simultaneous reactions generate gas-phase product can also be defeated by the pressure of reaction gas It transports and quickly escapes.

Claims (3)

1. a kind of crucible that crucible bottom is stepped is integrally formed by sidewall of crucible and crucible bottom group, it is characterised in that:Sidewall of crucible is in Hollow bevel is cylindrical, and it is in pipe angular cut to make mouth of pot, and crucible bottom inner face is stepped;The circular arc of wherein minimum ladder The minimum point of midpoint and sidewall of crucible, that is, pipe angular cut is to just, height of the sidewall of crucible minimum point away from minimum cascaded surface is 0.5 ~ 1 mm;Height of the peak of sidewall of crucible away from highest cascaded surface is 1.5 ~ 2.5 mm;The height of every grade of ladder is 1-2 mm;Pipe is oblique The tangent value of angle is 1 between face and horizontal plane where notch:3~1:1.
2. the crucible that crucible bottom according to claim 1 is stepped, which is characterized in that crucible bottom thinnest part and sidewall of crucible Thickness be 0.5 mm, a diameter of 10 ~ 17 mm of crucible bottom outer surface.
3. the crucible that crucible bottom according to claim 1 or 2 is stepped, which is characterized in that material is high purity aluminium oxide Or platinum.
CN201820369918.7U 2018-03-19 2018-03-19 The crucible that crucible bottom is stepped Active CN208043721U (en)

Priority Applications (1)

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CN208043721U true CN208043721U (en) 2018-11-02

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108279250A (en) * 2018-03-19 2018-07-13 沈阳环境科学研究院 The crucible and its application method that crucible bottom is stepped

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108279250A (en) * 2018-03-19 2018-07-13 沈阳环境科学研究院 The crucible and its application method that crucible bottom is stepped

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