CN106248553B - Based on gas osmosis to the characterizing method of plastic binded median surface structure - Google Patents
Based on gas osmosis to the characterizing method of plastic binded median surface structure Download PDFInfo
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- CN106248553B CN106248553B CN201610740980.8A CN201610740980A CN106248553B CN 106248553 B CN106248553 B CN 106248553B CN 201610740980 A CN201610740980 A CN 201610740980A CN 106248553 B CN106248553 B CN 106248553B
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- 238000000034 method Methods 0.000 title claims abstract description 29
- 239000004033 plastic Substances 0.000 title claims abstract description 15
- 239000002360 explosive Substances 0.000 claims abstract description 34
- 230000035699 permeability Effects 0.000 claims abstract description 30
- 239000011230 binding agent Substances 0.000 claims abstract description 28
- 239000000523 sample Substances 0.000 claims abstract description 7
- 238000012360 testing method Methods 0.000 claims abstract description 4
- 239000007789 gas Substances 0.000 claims description 63
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 239000013078 crystal Substances 0.000 claims description 4
- 230000008595 infiltration Effects 0.000 claims description 3
- 238000001764 infiltration Methods 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 230000005540 biological transmission Effects 0.000 claims description 2
- 238000009792 diffusion process Methods 0.000 claims description 2
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical group [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims description 2
- 229910001872 inorganic gas Inorganic materials 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- JDFUJAMTCCQARF-UHFFFAOYSA-N tatb Chemical compound NC1=C([N+]([O-])=O)C(N)=C([N+]([O-])=O)C(N)=C1[N+]([O-])=O JDFUJAMTCCQARF-UHFFFAOYSA-N 0.000 claims description 2
- 238000010998 test method Methods 0.000 claims description 2
- 238000011426 transformation method Methods 0.000 claims description 2
- 238000012512 characterization method Methods 0.000 abstract description 10
- 239000007767 bonding agent Substances 0.000 abstract description 3
- 238000011160 research Methods 0.000 abstract description 3
- 238000011161 development Methods 0.000 abstract description 2
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 3
- 239000002033 PVDF binder Substances 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 238000005474 detonation Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000002139 neutron reflectometry Methods 0.000 description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 238000000108 ultra-filtration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000009527 percussion Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000001485 positron annihilation lifetime spectroscopy Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000010345 tape casting Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N15/082—Investigating permeability by forcing a fluid through a sample
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N15/088—Investigating volume, surface area, size or distribution of pores; Porosimetry
Landscapes
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Testing Resistance To Weather, Investigating Materials By Mechanical Methods (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention discloses a kind of based on gas osmosis to the characterizing method of plastic binded median surface structure, includes the following steps:Step A:It uses gas molecule for probe, under certain pressure and temperature condition, tests the gas permeability coefficient of binder and the gas permeability coefficient of PBX that at least one explosive content is not zero;Step B:Using improved HIM models, the median surfaces PBX hole thickness is calculated in the gas permeability coefficient of the gas permeability coefficient and PBX of the binder measured in fit procedure A.This method is simple and practicable to PBX interfacial structure characterization techniques, it can be with the interfacial structure of PBX under quantitatively characterizing nanoscale, play an important roll for the development law of PBX interfacial structures under the conditions of research temperature, stress loading, effective way also is provided to the affecting laws of PBX interfacial structures to investigate different bonding agents.
Description
Technical field
The invention belongs to PBX structural characterization technical fields, and in particular to one kind is fried to plastic bonding based on gas osmosis
The characterizing method of medicine median surface structure.
Background technology
PBX is a kind of high filled composite materials using polymer plastic as continuous phase, high explosive crystal for dispersed phase, is
Important specific function material and structure member in weapon system have extensive in the detonation detonation train and main charge of weapon
Using.However the percussions such as temperature, stress during by machine-shaping and transport storage etc., PBX components interiors are very likely
Various forms of microstructure changes and interior damage aggregation are formed, the physicochemical property of PBX components is impacted, Explosive Parts are caused
Degradation, mechanical property degradation, the bearing capacity of doing work decline, or even macroscopic cracking and fracture failure occur, and then influence military
The safety and reliability of device.
The position that damage occurs in PBX includes:Explosive crystal is broken, polymeric binder fracture and explosive and bonding
Agent interfacial detachment.Wherein, the interface of explosive and binder is the position most easily damaged in PBX.Therefore, to the interfaces PBX
Micro-structure is characterized, and research PBX interface microstructures are to verify to damage shape in PBX with the Evolution of the factors such as temperature, stress
At the important channel of mechanism, also to solve, PBX is cracked to establish important foundation.Currently, can be used for characterizing PBX interface microstructures
Technology have very much, according to characterization scale can be divided into three classes.The first kind is macro-scale characterization method, including electronics and optics
Microscope.But microscope is only capable of the local pattern on observation surface, it can not quantitatively characterizing PBX internal structures.Second class is micron
Scale characterization method, predominantly tomoscan X-ray (CT).Third class be nanosecond yardstick surface features means, including the small angle of X-ray dissipate
Penetrate (SAXS), neutron small angle scattering (SANS), neutron reflection (NR), positron annihilation (PALS) etc..But above-mentioned characterization technique
In, the technology of the energy following micro-structures of quantitative description 10nm is still very deficient;Moreover, still not specifically for the table of PBX interfacial structures
Sign method.
To solve the above problems, this patent provides a kind of PBX interfacial structure characterization techniques permeated based on gas:With gas
Body molecule is probe, by testing the gas permeation property of PBX, explosive and binder interface structure in quantitatively characterizing PBX.Due to
Gas molecule size is generally less than 1nm, and transmittance process is influenced significantly by the defect sturcture of nanoscale, therefore suitable for characterization
Nanoscale interfacial structure in PBX.
Invention content
The object of the present invention is to provide a kind of based on gas osmosis to the characterization side of plastic binded median surface structure
Method, explosive and binder interface structure in quantitatively characterizing PBX.
In order to reach above-mentioned technique effect, the present invention takes following technical scheme:
It is a kind of based on gas osmosis to the characterizing method of plastic binded median surface structure, include the following steps:
Step A:It uses gas molecule for probe, under certain pressure and temperature condition, tests the gas infiltration of binder
The gas permeability coefficient for the PBX that coefficient and at least one explosive content are not zero;
Step B:Using improved HIM models, the gas permeability coefficient of the binder measured in fit procedure A and PBX's
The median surfaces PBX hole thickness is calculated in gas permeability coefficient.
Further technical solution is that the gas molecule is the inorganic gas for being not easy to condense.
Further technical solution is that the gas molecule is selected from helium, hydrogen, nitrogen or argon gas.
Further technical solution is that the test method of the gas permeability coefficient is constant volume transformation method or constant pressure transfiguration
Method;The feed pressure of gas is 0.2~0.5MPa;Temperature is 20~80 DEG C.
Further technical solution is that the mass fraction of explosive is not more than 10% in the PBX.
Further technical solution is the one kind of the explosive in the PBX in HMX, RDX or TATB;Explosive
Known to average-size.
Further technical solution is that the interfacial structure type of explosive and binder is in the improved HIM models
Hole, transmission form of the gas in interface is Knudsen diffusion, and explosive crystal is airtight.
Further technical solution is that the mathematic(al) representation of the improved HIM models is as follows:
φII=22/331/3φ'dθ (3)
Wherein, PrFor the ratio of the gas permeability coefficient of the gas permeability coefficient and binder of PBX;ΦdIt is explosive in PBX
Volume fraction;dpFor the diameter of explosive;T is the thickness of explosive and binder interface gap;λiIt is empty for explosive and binder interface
The ratio of the gas permeability coefficient of gap and the gas permeability coefficient of binder, R are gas constant, and T is temperature, MWFor gas probe
Molecular weight, PiFor the gas permeability coefficient of explosive and binder interface gap.
The gas permeability coefficient of PBX is measured by step A;The gas permeability coefficient of binder is tested by step A, when
When the volume fraction of explosive is 0, the gas permeability coefficient measured is the gas permeability coefficient of binder;Explosive and binder circle
The gas permeability coefficient in face gap is calculated by formula (9).
Further technical solution is that the feed pressure of the gas is 0.4MPa.
Compared with prior art, the present invention having advantageous effect below:
This method is simple and practicable to PBX interfacial structure characterization techniques, can be with the interface of PBX under quantitatively characterizing nanoscale
Structure plays an important roll the development law of PBX interfacial structures under the conditions of research temperature, stress loading, also not for investigation
Effective way is provided to the affecting laws of PBX interfacial structures with bonding agent.
Description of the drawings
Fig. 1 is scanning electron microscope (SEM) figure of PBX films prepared by embodiment 1.
Fig. 2 is the result figure that explosive and binder interface gap are fitted in embodiment 1.
Specific implementation mode
With reference to the embodiment of the present invention, the invention will be further elaborated.
Embodiment 1:
4g F2311 rubber is added in 96g ethyl acetate, is stirred 10 hours at 40 DEG C, it is 4wt% to obtain content
The ethyl acetate solution of F2311.The HMX that average grain diameter is 1.36 μm is added in ethyl acetate solution, is stirred 10 minutes, ultrasound
Dispersion 30 minutes, obtains the HMX suspension that content is respectively 0,0.04,0.2,0.32,0.4wt%.Using knife coating, will contain
Amount for 0,0.04,0.2,0.32, the HMX suspension of 0.4wt% be respectively coated on the porous ultrafiltration membrane table of Kynoar (PVDF)
Face, wet coating thickness are 120 μm.PVDF ultrafiltration membrane surface apertures are 15nm.PBX films are made in the solvent flashing at 30 DEG C.
It is measured through electron microscope, PBX film thicknesses are 1.1 μm, as shown in Fig. 1.
HMX volume fractions are respectively 0,1,5,8,10% in PBX films.With N2Molecule is probe, using constant pressure variable volume method,
At 0.4MPa, 20 DEG C, the gas permeability coefficient that measures PBX films is respectively 0.311,0.364,0.416,0.439,
0.455Barrer.Bring above-mentioned experiment parameter and the PBX film gas infiltration coefficients measured into improved HIM models (PBX
The gas permeability coefficient measured when HMX volume fractions are respectively 0% in film is the gas permeability coefficient of binder), fitting
Obtain the thickness t in explosive and binder interface gap for 2.2nm, degree of fitting R=0.9998, as a result as shown in Fig. 2.
Although reference be made herein to invention has been described for explanatory embodiment of the invention, and above-described embodiment is only this hair
Bright preferable embodiment, embodiment of the present invention are not limited by the above embodiments, it should be appreciated that people in the art
Member can be designed that a lot of other modification and implementations, these modifications and implementations will be fallen in principle disclosed in the present application
Within scope and spirit.
Claims (8)
1. it is a kind of based on gas osmosis to the characterizing method of plastic binded median surface structure, it is characterised in that including following
Step:
Step A:It uses gas molecule for probe, under certain pressure and temperature condition, tests the gas permeability coefficient of binder
The gas permeability coefficient for the PBX being not zero at least one explosive content;
Step B:Using improved HIM models, the gas of the gas permeability coefficient and PBX of the binder measured in fit procedure A
The median surfaces PBX hole thickness is calculated in infiltration coefficient;The mathematic(al) representation of the improved HIM models is as follows:
φII=22/331/3φ'dθ (3)
Wherein, PrFor the ratio of the gas permeability coefficient of the gas permeability coefficient and binder of PBX;ΦdThe body for being explosive in PBX
Fraction;dpFor the diameter of explosive;T is the thickness of explosive and binder interface gap;λiFor explosive and binder interface gap
The ratio of the gas permeability coefficient of gas permeability coefficient and binder, R are gas constant, and T is temperature, MWFor the molecule of gas probe
Amount, PiFor the gas permeability coefficient of explosive and binder interface gap.
2. it is according to claim 1 based on gas osmosis to the characterizing method of plastic binded median surface structure,
It is characterized in that the gas molecule is the inorganic gas for being not easy to condense.
3. it is according to claim 2 based on gas osmosis to the characterizing method of plastic binded median surface structure,
It is characterized in that the gas molecule is selected from helium, hydrogen, nitrogen or argon gas.
4. it is according to claim 1 based on gas osmosis to the characterizing method of plastic binded median surface structure,
It is characterized in that the test method of the gas permeability coefficient is constant volume transformation method or constant pressure variable volume method;The feed pressure of gas is
0.2~0.5MPa;Temperature is 20~80 DEG C.
5. it is according to claim 1 based on gas osmosis to the characterizing method of plastic binded median surface structure,
The mass fraction of explosive is not more than 10% in PBX described in being characterized in that.
6. it is according to claim 1 based on gas osmosis to the characterizing method of plastic binded median surface structure,
The one kind of the explosive in PBX in HMX, RDX or TATB described in being characterized in that;Known to the average-size of explosive.
7. it is according to claim 1 based on gas osmosis to the characterizing method of plastic binded median surface structure,
The interfacial structure type of explosive and binder is hole in improved HIM models described in being characterized in that, and gas is in interface
Transmission form is Knudsen diffusion, and explosive crystal is airtight.
8. it is according to claim 1 based on gas osmosis to the characterizing method of plastic binded median surface structure,
It is characterized in that the feed pressure of gas is 0.4MPa.
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