CN105372289B - The measurement modification method that a kind of energetic material apparent specific heat holds - Google Patents
The measurement modification method that a kind of energetic material apparent specific heat holds Download PDFInfo
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- CN105372289B CN105372289B CN201510817148.9A CN201510817148A CN105372289B CN 105372289 B CN105372289 B CN 105372289B CN 201510817148 A CN201510817148 A CN 201510817148A CN 105372289 B CN105372289 B CN 105372289B
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- 239000000463 material Substances 0.000 title claims abstract description 23
- 238000005259 measurement Methods 0.000 title claims abstract description 20
- 238000002715 modification method Methods 0.000 title claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 19
- 229910052594 sapphire Inorganic materials 0.000 claims abstract description 17
- 239000010980 sapphire Substances 0.000 claims abstract description 17
- 239000000126 substance Substances 0.000 claims abstract description 11
- 230000004580 weight loss Effects 0.000 claims abstract description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 3
- 208000016261 weight loss Diseases 0.000 claims description 9
- 238000012360 testing method Methods 0.000 claims description 6
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 3
- 230000007613 environmental effect Effects 0.000 claims description 2
- 238000012937 correction Methods 0.000 abstract description 2
- 229920002521 macromolecule Polymers 0.000 abstract 1
- 230000005945 translocation Effects 0.000 abstract 1
- 229920002121 Hydroxyl-terminated polybutadiene Polymers 0.000 description 2
- 239000003380 propellant Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 238000001938 differential scanning calorimetry curve Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000010058 rubber compounding Methods 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
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- Investigating Or Analyzing Materials Using Thermal Means (AREA)
Abstract
The present invention relates to the measurement modification methods that a kind of energetic material apparent specific heat holds, it is characterized in that, by measuring measured DSC TG differential calorimetrics thermal weight loss, the practical apparent specific heat varied with temperature of substance that parameter measured by amendment obtains holds, so as to obtain the practical actual value of Chinese energy material apparent specific heat appearance, specifically include：Energetic material style prepares, adjusts nitrogen flow rate, DSC TG curves are obtained with DSC TG translocations method, measure sapphire DSC TG curves, need correction tape temperature spot according to curvilinear trend selection, sample and sapphire rate of heat flow and weight are measured respectively, and eight steps of specific heat capacity of relevant temperature point are calculated using formula.The present invention is compared with the existing technology advantageous in that, has fully considered that Chinese energy material, macromolecule know thermal weight loss characteristic, and the method for providing versatility is corrected in the measurement for volatility variable specific heat coefficient.
Description
Technical field
The invention belongs to energetic material thermophysical parameter field of measuring technique, are related to a kind of amendment energetic material apparent specific heat
Hold the method for varying with temperature and measurement parameter being caused to change.
Background technology
Specific heat capacity is an important thermophysical parameter of substance.Utilize DSC (Differential Scanning
Calorisetry) method carrys out SPECIFIC HEAT CAPACITY, has the advantages that sample is few, speed is fast, easy to operate.This method is to substance ratio
The measurement of heat is mass conservation in visual substance heating process, and energetic material belongs to thermal weight loss section bar material, i.e.,：With temperature liter
It is high, it may appear that weightlessness, while its specific heat capacity can also change, thus obtained specific heat capacity does not meet the spy of substance in itself
Sign.This patent will be held by obtaining the practical apparent specific heat varied with temperature of substance to the revision of measured parameter.
Pervious in the prior art, " experimental study for waiting rubber Specific Heat Capacity " that Zhou Guibin etc. is delivered in the present invention《Generation
Boundary's rubber industry》2006,33(3):20-22；Tan Lianghong, Zhou Shuhua, Wang Jin, Zhang Younan deliver " differential scanning calorimeter exists
Application in rubber compounding research "《Extraordinary rubber product》2003,23(2):52-55；" the evaluation stability of explosive that Jia Xiangrui is delivered
With a kind of new method of compatibility "《War industry's journal》1995：Tri- documents of 85-88 are the comparison skills mostly concerned with the present invention
Art, but in this three documents, find no and close quantitatively calibrating thermal weight loss section bar material no-load voltage ratio thermal parameter measurement modification method
Report.
Invention content
Situation for the above-mentioned prior art, it is an object of the present invention to explore volatility energetic material Parameters Evolution rule
Rule, provides thermal weight loss section bar material Variable specific heat parameter measurement modification method, while also provide more accurate data for numerical simulation
And parameter.
Now present inventive concept and technical solution are described below：
The basic conception of the method for the present invention is, by under high pure nitrogen environment, to tested DSC heat flow versus temperatures curve-
The amendment of TG (Thermal Gravity Analysis) thermal weight loss-temperature curve obtains the practical hot-fluid that substance varies with temperature
Value and weight-loss ratio, parameter measured by amendment obtain the practical apparent specific heat varied with temperature of substance and hold, and contain energy material so as to obtain
The practical actual value of material, specifically includes following steps：
Step 1：Ready energetic material sample to be tested, shape are：0.5~1.5mm of thickness, a diameter of 5~8mm is (absolutely
.01mm is less than to error) the smooth disk in two sides；
Step 2：Measure quality m, the m ' of sapphire quality and sample；
Step 3：In high pure nitrogen atmosphere, flow velocity is measured using differential calorimetric method under conditions of being 30~50ml/min and tried
The blank baseline of sample environment；
Step 4：The DSC-TG curves of test piece are measured using DSC-TG combination methods under similary environmental condition.It will when filling sample
Light shake sample disc, it is good to be contacted between sample room, sample and disk；
Step 5：Under similarity condition sapphire DSC-TG curves are measured using DSC-TG combination methods；
Step 6：Several temperature spots are selected according to the trend of curve, flat part lacks reconnaissance 1-4, changes compared with steep part
For 4-6 point of multiselect point as modified temperature spot is needed, institute's reconnaissance amounts to n；
Step 7：According to its rate of heat flow and weight in n temperature spot of the DSC-TG curved measurements of institute's testing piece；
Step 8：According to its rate of heat flow and weight in n temperature spot of sapphire DSC-TG curved measurements；
Step 9：Specific heat capacity of the sample in relevant temperature point is calculated using formula (1)：
Wherein Cp、Cp' it is respectively sample and sapphire specific heat capacity under Current Temperatures, m, m ' they are respectively to be tried under Current Temperatures
Sample and sapphire quality,Sample and sapphire rate of heat flow respectively under Current Temperatures.
The present invention is compared with the existing technology advantageous in that：This method has fully considered energetic material/polymer substance
Thermal weight loss characteristic, for hot volatile material variable specific heat coefficient measurement correct provide versatility method.
Description of the drawings
Fig. 1：DSC curve
Fig. 2：TG curves
Specific embodiment
Below by taking HTPB propellant as an example, illustrate the measurement modification method that its apparent specific heat holds.
Step 1：The sample to be tested of ready HTPB propellant, shape thicknesses 1mm, (absolute error is small by a diameter of 6mm
In .01mm) the smooth disk in two sides；
Step 2：Measure quality m, the m ' of sapphire quality and sample；
Step 3：In high pure nitrogen atmosphere, flow velocity utilizes differential calorimetric method measurement sample ring under conditions of being 40ml/min
The blank baseline in border；
Step 4：The DSC-TG curves of test piece are measured using DSC-TG combination methods under similarity condition；
Step 5：Under similarity condition sapphire DSC-TG curves are measured using DSC-TG combination methods；
Step 6：Several temperature spots are selected according to the trend of curve, flat part selects 3 points, changes and select 4 compared with steep part
For a point as modified temperature spot is needed, selected temperature spot amounts to 7；
Step 7：According to its rate of heat flow and weight in 7 temperature spots of the DSC-TG curved measurements of institute's testing piece；
Step 8：According to its rate of heat flow and weight in 7 temperature spots of sapphire DSC-TG curved measurements；
Step 9：Specific heat capacity of the sample in relevant temperature point is calculated using formula (1).
The apparent thermal capacitance variation with temperature value of 1 sample of table
| Temperature/DEG C | Initial value Cp | Weight-loss ratio | Correction value Cp ' |
| 25.85 | 2.14 | 0 | 2.14 |
| 177.24 | 2.28 | 0 | 2.28 |
| 237.79 | 2.53 | 0 | 2.53 |
| 328.62 | 2.25 | 0.3 | 3.22 |
| 358.90 | 3.16 | 0.35 | 4.86 |
| 378.45 | 3.38 | 0.4 | 5.63 |
| 400.35 | 3.99 | 0.45 | 7.25 |
Claims (2)
1. a kind of measurement modification method that energetic material apparent specific heat holds, it is characterised in that：It is right by under high pure nitrogen environment
The amendment of tested DSC heat flow versus temperatures curve-TG thermal weight losses-temperature curve obtains the practical heat flow value that substance varies with temperature
And weight-loss ratio, parameter measured by amendment obtains the practical apparent specific heat varied with temperature of substance and holds, so as to obtain energetic material
Practical actual value, specifically include following steps：
Step 1：Ready energetic material sample to be tested；
Step 2：Measure quality m, the m ' of sapphire quality and sample；
Step 3：In high pure nitrogen atmosphere, flow velocity utilizes differential calorimetric method measurement sample ring under conditions of being 30~50ml/min
The blank baseline in border；
Step 4：The DSC-TG curves of test piece are measured using DSC-TG combination methods under similary environmental condition, gently to be shaken when filling sample
Sample disc, it is good to be contacted between sample room, sample and disk；
Step 5：Under similarity condition sapphire DSC-TG curves are measured using DSC-TG combination methods；
Step 6：Several temperature spots are selected according to the trend of curve, flat part lacks reconnaissance 1-4, changes compared with steep part multiselect
For 4-6 point of point as modified temperature spot is needed, institute's reconnaissance amounts to n；
Step 7：According to its rate of heat flow and weight in n temperature spot of the DSC-TG curved measurements of institute's testing piece；
Step 8：According to its rate of heat flow and weight in n temperature spot of sapphire DSC-TG curved measurements；
Step 9：Sample is calculated using formula (1) in the apparent specific heat of relevant temperature point to hold：
Wherein Cp、Cp' it is respectively sample and sapphire apparent specific heat appearance under Current Temperatures, it is tried under m, m ' respectively Current Temperatures
Sample and sapphire quality,Sample and sapphire rate of heat flow respectively under Current Temperatures.
2. the measurement modification method that a kind of energetic material apparent specific heat according to claim 1 holds, it is characterised in that：It is described
Energetic material sample to be tested its shape be：0.5~1.5mm of thickness, a diameter of 5~8mm, absolute error is less than the two of .01mm
The smooth disk in face.
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| CN201510817148.9A CN105372289B (en) | 2015-11-21 | 2015-11-21 | The measurement modification method that a kind of energetic material apparent specific heat holds |
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| CN201510817148.9A CN105372289B (en) | 2015-11-21 | 2015-11-21 | The measurement modification method that a kind of energetic material apparent specific heat holds |
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| Publication Number | Publication Date |
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| CN105372289A CN105372289A (en) | 2016-03-02 |
| CN105372289B true CN105372289B (en) | 2018-06-08 |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1136802A1 (en) * | 2000-03-23 | 2001-09-26 | TA Instruments, Inc. | Modulated differential scanning calorimeter |
| CN101308107A (en) * | 2007-05-16 | 2008-11-19 | 比亚迪股份有限公司 | Process for determining thermoconductivity |
| CN101915774A (en) * | 2010-08-09 | 2010-12-15 | 中国计量科学研究院 | Method for Determination of Melting Point of Organic Substances Using Differential Scanning Calorimetry |
| CN202814902U (en) * | 2012-09-21 | 2013-03-20 | 西安建筑科技大学 | Testing device for thermal diffusivity of bituminous mixture |
| CN205333549U (en) * | 2015-12-24 | 2016-06-22 | 深圳市建筑科学研究院股份有限公司 | Compound phase change material latent heat survey device |
-
2015
- 2015-11-21 CN CN201510817148.9A patent/CN105372289B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1136802A1 (en) * | 2000-03-23 | 2001-09-26 | TA Instruments, Inc. | Modulated differential scanning calorimeter |
| CN101308107A (en) * | 2007-05-16 | 2008-11-19 | 比亚迪股份有限公司 | Process for determining thermoconductivity |
| CN101915774A (en) * | 2010-08-09 | 2010-12-15 | 中国计量科学研究院 | Method for Determination of Melting Point of Organic Substances Using Differential Scanning Calorimetry |
| CN202814902U (en) * | 2012-09-21 | 2013-03-20 | 西安建筑科技大学 | Testing device for thermal diffusivity of bituminous mixture |
| CN205333549U (en) * | 2015-12-24 | 2016-06-22 | 深圳市建筑科学研究院股份有限公司 | Compound phase change material latent heat survey device |
Non-Patent Citations (3)
| Title |
|---|
| 材料比热容测试国内外试验方法比较;张红菊 等;《理化检验-物理分册》;20141231;第50卷(第10期);741-743 * |
| 用DSC法测量U0.77Zr0.23合金的热熔;李永静 等;《原子能科学技术》;19960731;第30卷(第4期);312-318 * |
| 用DSC测量复铜板玻璃化转变区的比热容;曾春莲 等;《广州化工》;20101231;第38卷(第12期);204-206 * |
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