CN104458887B - The micro migration component detection method of heat insulation layer in propellant bonding system - Google Patents
The micro migration component detection method of heat insulation layer in propellant bonding system Download PDFInfo
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- CN104458887B CN104458887B CN201310421816.7A CN201310421816A CN104458887B CN 104458887 B CN104458887 B CN 104458887B CN 201310421816 A CN201310421816 A CN 201310421816A CN 104458887 B CN104458887 B CN 104458887B
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Abstract
The present invention is the micro migration component detection method of heat insulation layer in a kind of propellant bonding system for the lossless static analysis of space flight polymer chemistry fuel.Detecting step is:Sample preparation, condition are chosen, collection of illustrative plates gathers, data parsing；During sample preparation, the bonding test specimen of heat insulation layer/lining/propellant is obtained, fresh bonding plane is cut with blade, is made by sample product；When condition is chosen, detection object is the micro migration component of heat insulation layer/lining bonding plane, and detection device is time of flight secondary ion massspectrometry instrument；Collection of illustrative plates acquisition alternative condition be：Primary ion source, voltage threshold, imaging mode, target current value, vacuum state, acquisition time, ion mode, correction ion；It utilizes time of flight secondary ion massspectrometry instrument, is parsed by collection of illustrative plates acquisition and data, carries out qualitative determination and semi-quantitative analysis to heat insulation layer migration component, and obtains its distribution information.The present invention also have the advantages that it is qualitative accurately, collection of illustrative plates it is directly perceived.
Description
Technical field
The present invention relates to a kind of SIMS analysis method of space flight polymer chemistry fuel, specifically one kind pushes away
The micro migration component detection method of heat insulation layer into agent bonding system.
Background technology
In solid propellant/lining/heat insulation layer bonding system, heat insulation layer migration component is directly related to interfacial adhesion
Can, thus need to carry out qualitative and quantitative detection to it.In the prior art, still examined for migrating component known to heat insulation layer
It surveys, and for the detection of the micro migration component of the unknown migration component of heat insulation layer, particularly heat insulation layer, then without ready-made technology.
The content of the invention
The invention aims to provide heat insulation layer in a kind of propellant bonding system micro migration component detection method, it
It can intuitively realize the qualitative and quantitative detection of the micro migration component of heat insulation layer, effectively evaluate heat insulation layer and migrate component in thermal insulation
Distribution in layer and lining.
The technical scheme is that：Design a kind of micro migration component detection side of heat insulation layer in propellant bonding system
Method, including following four step:Sample preparation, condition are chosen, collection of illustrative plates gathers, data parsing, it is characterised in that：In sample preparation
Stage obtains the bonding test specimen of heat insulation layer/lining/propellant, cuts fresh bonding plane with blade, be cut into smooth flake and examined
Sample；The stage is chosen in condition, detection object is the micro migration component of heat insulation layer/lining bonding plane, and detection device is flight
Time ion microprobe (TOF-SIMS)；Collection of illustrative plates acquisition alternative condition be：Primary ion source, voltage threshold, imaging side
Formula, target current value, vacuum state, acquisition time, ion mode, correction ion；In data resolution phase, collection of illustrative plates is compareed, is passed through
Analysis obtains qualitative judgement, semi-quantitative data and the distribution in heat insulation layer and lining of heat insulation layer migration component.
In sample preparation steps, smooth flake by inspection sample specification is no less than 500 no more than 5mm, area for thickness ×
500 μm²。
In collection of illustrative plates acquisition phase, primary ion source Bi3+Ion source or C60Ion source, voltage threshold are 25 keV, into
Image space formula is imaged for high-quality resolution rate surface composition, and target current value is 0.2pA-0.3 pA, and vacuum degree is not less than 1 × 10–7
Mbar, ion acquisition time are 1-30min, and ion mode is positive/negative ion mode, and ion nucleocytoplasmic ratio uses H+、CH3 +、C2H5 +
Correction.
The advantageous effects of the present invention：Due in sample preparation steps, directly acquiring heat insulation layer/lining/propellant
Smooth flake is made by sample product in bonding test specimen, thus sample making process is simple.Simultaneously because when detection device is flight
Between ion microprobe (TOF-SIMS), thus detection sensitivity is high, can reach the ppm even magnitude of ppb, can carry out absolutely
Thermosphere migration component zero judges, can also carry out micro-area composition imaging and ANALYSIS ON DEPTH PROFILES.It gathers and uses additionally, due to collection of illustrative plates
High-quality resolution rate surface composition imaging mode, thus be conducive to the migration group to heat insulation layer/lining/propellant bonding system
It is point qualitative, and provide technical support to establish heat insulation layer migration component common detection methods.The present invention also have it is qualitative it is accurate,
The advantages of collection of illustrative plates is directly perceived.
Description of the drawings
Fig. 1 is the migration component mass spectrogram of EPDM heat insulation layer under positive ion mode, and in Fig. 1, abscissa is ion
Mass-to-charge ratio；Ordinate is ion intensity of flow；C8H8For styrene, C8H8O is acetophenone, C9H12O is phenylpropanol.
Fig. 2 is that EPDM heat insulation layer migrates component mass spectrogram under negative ion mode, and in Fig. 2, abscissa is the matter of ion
Lotus ratio；Ordinate is ion intensity of flow；C16H32O2For palmitic acid, C18H36O2For stearic acid, C24H30N2For 1,2- dihydro -2,
2,4-trimethylquinoline dimer.
Fig. 3 is EPDM heat insulation layer/fourth hydroxyl lining bonding interface migration constituent mass distribution map, in Fig. 3, from left to right
It is:Bonding plane photo, palmitic acid and stearic acid, 1,2- dihydro-2,2,4-trimethylquinoline dimers, acetophenone.
Specific embodiment
Dividing three groups with reference to embodiment, the present invention is further described.
First group, EPDM heat insulation layer migrates the qualitative determination of component.
Step 1, sample preparation：In sample preparation steps, the viscous of EPDM heat insulation layer/fourth hydroxyl lining/propellant is obtained
Test specimen is connect, fresh bonding plane is cut with blade, smooth flake is cut by sample product, is not more than by inspection sample specification for thickness
5mm, area are no less than 500 × 500 μm 2.
Step 2, condition are chosen：The stage is chosen in condition, detection object is EPDM heat insulation layer/lining bonding plane
Micro migration component, detection device are time of flight secondary ion massspectrometry instrument (TOF-SIMS)；
Step 3, collection of illustrative plates acquisition：Collection of illustrative plates acquisition alternative condition be：Primary ion source, voltage threshold, imaging mode, target
Current value, vacuum state, acquisition time, ion mode, correction ion.In collection of illustrative plates acquisition phase, primary ion source Bi3+Ion
Source or C60Ion source, voltage threshold are 25 keV, and target current value is 0.2pA-0.3 pA, and vacuum degree is not less than 1 × 10–7
Mbar, ion acquisition time are 1-30min, and ion mode is positive/negative ion mode, and ion nucleocytoplasmic ratio uses hydrogen ion H+、CH3 +、C2H5 +Correction.
Step 4, data parsing：It is formed with reference to the element that component may be migrated in EPDM heat insulation layer, what is gathered
The accurate molecular weight of migration component fragment is found in lining mass spectrogram, and retrieves its element composition, confirmation migration component.
In Fig. 1, the element retrieved forms C8H8,C8H8O and C9H12O is respectively styrene, acetophenone and phenylpropanol,
Cumyl peroxide decomposition product can be attributed to, due to detecting styrene, benzene in fourth hydroxyl lining, EPDM heat insulation layer
Ethyl ketone and phenylpropanol quasi-molecular ions are only with the addition of oxidation diisopropylbenzene (DIPB), non-adhesive system in EPDM heat insulation layer in actual formula
Fourth hydroxyl lining in and there is no the component, therefore illustrate that the cumyl peroxide decomposition product in EPDM heat insulation layer migrates
Fourth hydroxyl lining is arrived, the decomposition of the raw material cumyl peroxide in heat insulation layer.
In Fig. 2, the element composition retrieved is C16H32O2And C18H36O2Quasi-molecular ions, be respectively stearic acid and palmitic acid,
Stearic acid and palmitic acid only are with the addition of in EPDM heat insulation layer in actual formula, are not deposited in the fourth hydroxyl lining of non-adhesive system
In the component, illustrate that the stearic acid in EPDM heat insulation layer and palmitic acid have been moved in lining, from heat insulation layer
Raw material.
According to Fig. 2 it can be seen that there are C in lining, heat insulation layer24H30N2Quasi-molecular ions, be 1,2- dihydros-2,2,4-
The polymeric dimer fragment of trimethylquinoline, is attributed to 1,2- dihydros-2,2,4-trimethylquinoline condensate dimer,
1,2- dihydros-2,2 only are with the addition of in EPDM heat insulation layer in actual formula, and 4-trimethylquinoline condensate dimer is non-
In the fourth hydroxyl lining of bonding system and there is no the component, illustrate the anti-aging agent 1 in heat insulation layer, 2- dihydros-2,2,4-front three
Base quinoline condensate has been moved in lining, derives from the raw material 1 of heat insulation layer, 2- dihydros-2,2,4-trimethylquinoline
Condensate.
Therefore, it is determined that the migration component in heat insulation layer is cumyl peroxide decomposition product styrene, acetophenone and phenylpropyl alcohol
Alcohol, stearic acid, palmitic acid, 1,2- dihydro-2,2,4-trimethylquinoline condensate dimers.It is respectively derived from heat insulation layer
In raw material cumyl peroxide, stearic acid and palmitic acid, 1,2- dihydro-2,2,4-trimethylquinoline condensates.
Second group, EPDM heat insulation layer migration component sxemiquantitative in heat insulation layer/lining/propellant bonding system.
Step 1, sample preparation：In sample preparation steps, the viscous of EPDM heat insulation layer/fourth hydroxyl lining/propellant is obtained
Test specimen is connect, fresh bonding plane is cut with blade, smooth flake is cut by sample product, is not more than by inspection sample specification for thickness
5mm, area are no less than 500 × 500 μm 2.
Step 2, condition are chosen：The stage is chosen in condition, detection object is EPDM heat insulation layer/fourth hydroxyl lining bonding
The micro migration component in face, detection device are time of flight secondary ion massspectrometry instrument (TOF-SIMS)；
Step 3, collection of illustrative plates acquisition：Collection of illustrative plates acquisition alternative condition be：Primary ion source, voltage threshold, imaging mode, target
Current value, vacuum state, acquisition time, ion mode, correction ion.In collection of illustrative plates acquisition phase, primary ion source Bi3+Ion
Source or C60Ion source, voltage threshold are 25 keV, and target current value is 0.2pA-0.3 pA, and vacuum degree is not less than 1 × 10–7
Mbar, ion acquisition time are 1-30min, and ion mode is positive/negative ion mode, and ion nucleocytoplasmic ratio uses hydrogen ion H+、CH3 +、C2H5 +Correction.
Step 4, data parsing：According to collection of illustrative plates, using CH peak intensities as ratio, heat insulation layer migration component mass spectrum peak intensity
Degree is normalized, and acquires EPDM heat insulation layer and moves to migration component relative quantity in lining.
Heat insulation layer moves to the Secondary Ion Mass Spectrometry figure relative peak intensities (%) of component in lining in 1 bonding system of table
| Migrate component | Stearic acid and palmitic acid total amount | Cumyl peroxide decomposition product | 1,2- dihydro-2,2,4-trimethylquinoline condensates |
| Heat insulation layer | 8.88 | 177.25 | 1.48 |
| Lining | 2.29 | 30.25 | 0.51 |
3rd group, in heat insulation layer/lining/propellant bonding system, EPDM heat insulation layer migrate component in heat insulation layer and
Distribution in lining.
Step 1, sample preparation：In sample preparation steps, the viscous of EPDM heat insulation layer/fourth hydroxyl lining/propellant is obtained
Test specimen is connect, fresh bonding plane is cut with blade, smooth flake is cut by sample product, is not more than by inspection sample specification for thickness
5mm, area are no less than 500 × 500 μm 2.
Step 2, condition are chosen：The stage is chosen in condition, detection object is EPDM heat insulation layer/fourth hydroxyl lining bonding
The micro migration component in face, detection device are time of flight secondary ion massspectrometry instrument (TOF-SIMS)；
Step 3, collection of illustrative plates acquisition：Collection of illustrative plates acquisition alternative condition be：Primary ion source, voltage threshold, imaging mode, target
Current value, vacuum state, acquisition time, ion mode, correction ion.In collection of illustrative plates acquisition phase, primary ion source Bi3+Ion
Source or C60Ion source, voltage threshold are 25 keV, and imaging mode is imaged for high-quality resolution rate surface composition, and target current value is
0.2pA-0.3 pA, vacuum degree are not less than 1 × 10–7 Mbar, ion acquisition time be 1-30min, ion mode for it is positive/negative from
Subpattern, ion nucleocytoplasmic ratio use hydrogen ion H+、CH3 +、C2H5 +Correction.
Step 4, data parsing：The secondary ion by mass spectrum separation sample is collected, to the ion imaging of sample surfaces,
Obtain surface distribution map of the migration component in lining and heat insulation layer.
Fig. 3 reflected migration component stearic acid and palmitic acid, 1,2--2,2,4-trimethylquinolines of dihydro condensate,
Distribution of the acetophenone in EPDM heat insulation layer and fourth hydroxyl lining.
Claims (2)
1. a kind of micro migration component detection method of heat insulation layer in propellant bonding system, including following four step:Sample system
Standby, condition is chosen, collection of illustrative plates gathers, data parsing, it is characterised in that：In sample preparation steps, heat insulation layer/lining/propulsion is obtained
The bonding test specimen of agent cuts fresh bonding plane with blade, is cut into smooth flake by sample product；Stage, detection are chosen in condition
Object is the micro migration component of heat insulation layer/lining bonding plane, and detection device is time of flight secondary ion massspectrometry instrument (TOF-
SIMS)；In collection of illustrative plates acquisition phase, the alternative condition of collection of illustrative plates acquisition is：Primary ion source, voltage threshold, imaging mode, target current
Value, vacuum state, acquisition time, ion mode, correction ion, wherein, primary ion source Bi3+Ion source or C60Ion
Source, voltage threshold are 25 keV, and imaging mode is imaged for high-quality resolution rate surface composition, and target current value is 0.2pA-0.3
PA, vacuum degree are not less than 1 × 10–7 Mbar, ion acquisition time be 1-30min, ion mode be positive/negative ion mode, ion
Nucleocytoplasmic ratio uses H+、CH3 +、C2H5 +Correction；In data resolution phase, collection of illustrative plates is compareed, heat insulation layer migration component is obtained by analyzing
Qualitative judgement, semi-quantitative data and the distribution in heat insulation layer and lining.
2. the micro migration component detection method of heat insulation layer in propellant bonding system according to claim 1, it is characterized in that：
In sample preparation steps, smooth flake is that thickness is not more than 5mm by inspection sample specification, and area is no less than 500 × 500 μm
²。
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101713762A (en) * | 2008-10-07 | 2010-05-26 | 中国科学院大连化学物理研究所 | Method for identifying and detecting halogenated hydrocarbons |
| CN102333551A (en) * | 2009-02-27 | 2012-01-25 | 宝洁公司 | Method for improving the barrier properties of a nonwoven |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101713762A (en) * | 2008-10-07 | 2010-05-26 | 中国科学院大连化学物理研究所 | Method for identifying and detecting halogenated hydrocarbons |
| CN102333551A (en) * | 2009-02-27 | 2012-01-25 | 宝洁公司 | Method for improving the barrier properties of a nonwoven |
Non-Patent Citations (1)
| Title |
|---|
| 丁羟推进剂粘接体系中的组分迁移;尹华丽等;《固体火箭技术》;20071031;416页第1段 * |
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