CN106018250A - Method for comprehensive assessment of reasons of irradiation ageing damage of nuclear power engineering plastics - Google Patents
Method for comprehensive assessment of reasons of irradiation ageing damage of nuclear power engineering plastics Download PDFInfo
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Abstract
The invention relates to a method for comprehensive assessment of reasons of irradiation ageing damage of nuclear power engineering plastics. The method comprises the steps of performing physical and mechanical property testing of polymer materials, and preliminarily observing macroscopic performance aging conditions of the materials after irradiation; performing morphological observation of aging products, and determining fracture reasons of the aging products to be ductile fracture, general brittle fracture and dissociative type fracture and the like in combination with testing results of physical and mechanical properties; adopting one or more of atlas and thermal analysis detection means to test stretch fracture surfaces and the inside of the materials and the like, and determining changing conditions of crystallinity inside the materials; synthesizing multiple detection and analysis means to perform system analysis and research on an aging mode of the aging materials, and finally determining the reasons of irradiation ageing damage of the engineering plastics in combination with fracture appearance observation and crystallinity analysis results. After comprehensive assessment on performances of valve material polyether-ether-ketone for nuclear power under ray irradiation conditions, the reasons of aging damage of the polyether-ether-ketone material can be determined accurately, and thus reasonable quality evaluation and failure prevention are performed.
Description
Technical field
The invention belongs to Material for nuclear power equipment detection technique field, be specifically related to a kind of nuclear power engineering plastics radiation aging
The synthetic judgement of damage reason, especially relates to the sentencing of radiation aging damage reason of a kind of valve polyetheretherketonematerials materials
Determine method.
Background technology
Since last century the fifties, nuclear energy power generation due to its uniqueness advantage and more and more by countries in the world
Attention, along with nuclear energy uses deeply and the increase of nuclear power station quantity, in nuclear power, the problem of aging of equipment causes people the most day by day
Concern.China's many places nuclear power station puts into operation the history of more than ten years, although the operation time is the longest, but faces
If the series of problems such as the ageing of performance of lay-by material, Damage and Failure.China is just planning the safety of original nuclear power plant to make at present
Bringing up to 60 years from 40 years with the time limit, the increase of following active time will make these problems the most prominent, become and affect nuclear power
The big hidden danger of the one of security of system of standing stable operation.Requiring in domestic nuclear safety codes " nuclear power plant design safety regulation " must be right
Nuclear power plant's material therefor quality is identified, with guarantee its within the whole phase in design and operation longevity properly functioning, when predicted operation
Between and design basis accident during can ensure that it is used safely.
In nuclear power station, the application of nonmetallic materials widely, including valve, pipeline, electric insulation system etc..Once
There is ageing of performance problem in material, will cause its place parts, or even the damage of whole equipment, can the control of initiated core power station time serious
The failure accidents of system processed, causes great manpower and materials to lose.Therefore, the selection of nonmetallic materials and superior in quality determine
Nuclear power control system and the service life of transmission system.The mechanics that high performance engineering plastics (such as polyether-ether-ketone) has excellence is special
Property and good radiation-resistant property, the most selected as nuclear power valve material.But in the military service operating mode that nuclear power station is complicated
In, polyetheretherketonematerials materials still is possible to occur because of the effect of the environmental conditions such as irradiation, heat, oxygen that ageing of performance even lost efficacy feelings
Condition, causes nuclear power plant's control system generation abnormal accident, brings significant damage to country and society.But currently for nuclear power with poly-
The radiation aging damage research of ether ether ketone engineering plastics does not has systematic characterization method and analysis system, it is impossible to it by irradiation shadow
Ring and Aging Damage reason accurately judges.Therefore, it is necessary to the engineering plastics in nuclear power plant are carried out radiation-resistant property and
The comprehensive of agine mechaism is analyzed and evaluation.The utilization in nuclear power generating equipment of the polyetheretherketone engineering plastics is not only carried by result of study
For important aging evaluation foundation, and to nuclear power, thermoelectricity, chemical industry engineering plastics in the Performance Evaluation of complex condition and mistake
Effect prevention also has important reference value.
Summary of the invention
The present invention is directed to problem present in background technology, it is proposed that one can be with system, judge nuclear power accurately and efficiently
Assessment method with polyetheretherketonematerials materials radiation aging damage reason.
The nuclear power decision method of polyetheretherketonematerials materials radiation aging damage reason that the present invention proposes, described nuclear power recruitment
Engineering plastics is polyetheretherketonematerials materials, specifically comprises the following steps that
Step one: detect the physical and mechanical property of the polyetheretherketonematerials materials after x ray irradiation x, analyzes it at different irradiation
The situation of change of physical and mechanical property before and after condition process, the situation of change of described physical and mechanical property includes: density of material is
No change, whether the tensile strength of material degenerates；
Step 2: outward appearance and the stretching fracture microscopic appearance to the polyetheretherketonematerials materials after x ray irradiation x, uses said three-dimensional body formula to show
Micro mirror (3DSM) and scanning electron microscope (SEM) are observed, and the physical and mechanical property test result of integrating step one, to spoke
Polyetheretherketonematerials materials tension failure form after according to carries out preliminary judgement；Tension failure pattern is divided into 3 kinds: ductile rupture, general
Brittle fracture and dissociative type fracture；
Step 3: on the basis of step 2 tentatively judges, uses infrared spectrum (FTIR) or thermal performance analysis further
(DSC) one or more in detection means, to inside and outside polyetheretherketonematerials materials after predose, stretching fracture position carry out microcosmic table
Levy analysis and test, so that it is determined that polyetheretherketonematerials materials situation of change of degree of crystallinity in irradiation process；
Step 4: on the basis of step 3, recycling infrared spectrum (FTIR), Raman spectrum (Raman), scanning electron microscope
(SEM) and energy spectrum analysis (EDS) detection means, integrating step two and the analysis result of step 3, determine that polyether-ether-ketone is irradiated
Aging Damage reason in journey；The reason causing Aging Damage is broadly divided into 2 kinds: oxidation reaction and crosslinking reconstruct.
In step 2 of the present invention:
3DSM and SEM is used to observe overall pattern and the stretching fracture microscopic appearance of polyetheretherketonematerials materials after predose, by difference
Observed result under radiation parameter contrasts, it is judged that the fracture mode belonging to polyetheretherketonematerials materials；
If the feature of stretching fracture is: Tensile fracture is uneven, short texture, there is the structures such as circular dimple, edge with
Corrugated lines；Then fracture mode is ductile rupture；
If the feature of stretching fracture is: Tensile fracture is concordant, compact structure, micro-crack or radial crack occur；Then rupture mould
Formula is general brittle fracture；
If the feature of stretching fracture is: exist circular or semicircular smooth concordant, it exists strip cracking lines, and split
Stricture of vagina propagation direction is consistent, can be also found that tongue pattern form crackle simultaneously；Then fracture mode is dissociative type fracture.
In step 3 of the present invention:
Microscopic sdIBM-2+2q.p.approach analysis is carried out for the polyetheretherketonematerials materials after predose, uses FTIR spectrum to analyze its microstructure, if
1305 cm-1(the bending vibration peak of agraphitic carbon skeleton) and 1288 cm-1The intensity at (the antisymmetric stretching vibration peak of diphenyl ether)
Ratio raises；Use DSC that hot property is analyzed simultaneously, find that inner molten enthalpy declines, it is determined that its Aging Damage causes
The degree of crystallinity of polyetheretherketonematerials materials reduces；Otherwise, then crystal region change is little.
In step 4 of the present invention:
For step 3 determines the polyetheretherketonematerials materials that degree of crystallinity reduces, FTIR and Raman is used to analyze its characteristic group
And carbon backbone structure, use SEM to observe its microscopic appearance；If collection of illustrative plates finds oxide group characteristic peak, microscopic appearance occurs
The results such as pore, it is determined that its Aging Damage reason is oxidation reaction；
For determining the polyetheretherketonematerials materials that degree of crystallinity reduces in step 3, if finding in collection of illustrative plates, molecular carbon framing structure changes,
Oxide group characteristic peak is without new change；In microscopic appearance, brittle zone ratio increases, without notable air hole structure, it is determined that it is old
Change damage reason for crosslinking reconstruct.
The beneficial effects of the present invention is:
1, this method fully utilizes various modern analytical tool and characterizing method, can be accurately judged to nuclear power polyethers ether
Macroscopical radiation aging phenomenon of ketone material and corresponding microstructure micromechanism of damage.
2, this method with system, the Aging Damage reason that effectively finds nuclear power polyetheretherketonematerials materials, thus can be entered
Row specific aim biometry and Failure prevention.
3, other equipment engineering materials are utilized and performance rating by this method nuclear power, thermoelectricity, the effective of petrochemical field
Also there is important reference value.
Accompanying drawing explanation
Fig. 1 is the stretching force value deformation curve figure of polyetheretherketonematerials materials before and after one group of electron beam irradiation shown in embodiment 1, its
In: (a) is the force value deformation pattern of predose material, and (b) is the force value deformation pattern of material after irradiation；
Fig. 2 is the density measurement result figure of polyetheretherketonematerials materials before and after electron beam irradiation shown in embodiment 1；
Fig. 3 is the tensile sample shape appearance figure of the ketone material of electron beam irradiation polyethers prior ether shown in embodiment 1, wherein: (a) is stretching examination
Sample fracture apperance, (b) is tensile sample matrix pattern；
Fig. 4 is the polyether-ether-ketone stretching fracture microscopic appearance after one group of electron beam irradiation shown in embodiment 1, wherein: (a) is fracture
Playing knick point microscopic appearance, (b) is fracture entirety pattern, and (c) is tongue crack morphology；
Fig. 5 is the infrared spectrogram of polyetheretherketonematerials materials before and after electron beam irradiation shown in embodiment 1；
Fig. 6 is the thermal performance test figure of polyetheretherketonematerials materials before and after electron beam irradiation shown in embodiment 1；
Fig. 7 is the Raman spectrogram of polyetheretherketonematerials materials before and after electron beam irradiation shown in embodiment 1, wherein: (a) is predose material
Material Raman spectrogram, (b) is material Raman spectrogram after irradiation；
Fig. 8 is the stretching force value deformation curve of polyetheretherketonematerials materials before and after one group of gamma-ray irradiation shown in embodiment 2, wherein: (a)
For the force value deformation pattern of predose material, (b) is the force value deformation pattern of material after irradiation；
Fig. 9 is the microscopic appearance figure of the stretching fracture of polyetheretherketonematerials materials after gamma-ray irradiation shown in embodiment 2, wherein: (a) is
Overall pattern, (b) is the face microscopic appearance that dissociates, and (c) is the face crack deformation pattern that dissociates；
Figure 10 is the infrared spectrogram of polyetheretherketonematerials materials before and after gamma-ray irradiation shown in embodiment 2；
Figure 11 is the stretching force value curve of polyetheretherketonematerials materials before and after gamma-ray irradiation under different temperatures shown in embodiment 3, wherein:
A () is the force value deformation pattern of predose material, (b) is the force value deformation pattern of material after 80 DEG C of irradiation；
Figure 12 is the microscopic appearance figure of the stretching fracture of polyetheretherketonematerials materials after the shown 80 DEG C of gamma-ray irradiations of embodiment 3, wherein:
A () is overall pattern, (b) is the face microscopic appearance that dissociates, and (c) amplifies pattern for the facial cleft stricture of vagina that dissociates；
Figure 13 is the infrared spectrogram of polyetheretherketonematerials materials before and after gamma-ray irradiation under different temperatures shown in embodiment 3；
Figure 14 is the thermal performance analysis figure of polyetheretherketonematerials materials after the shown 80 DEG C of gamma-ray irradiations of embodiment 3.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is expanded on further.Should be understood that these embodiments are merely to illustrate the present invention
Rather than restriction the scope of the present invention.In addition, it is to be understood that after having read the content that the present invention lectures, people in the art
The present invention can be made various changes or modifications by member, and these equivalent form of values fall within the application appended claims equally and limited
Scope.
Embodiment 1: the Aging Damage reason under the conditions of irradiation dose and analysis
Fig. 1 show the stretching force value deformation curve of polyether-ether-ketone (PEEK) before and after electron beam irradiation.Can be seen that drawing of PEEK
Stretch curve and belong to the saddle type curve of standard, experience elastic deformation, surrender (one-tenth neck), the generation rank such as large deformation and strain hardening
Section (Fig. 1 (a)).Stress at the elastic deformation phase material of material quickly increases, and strain variation is comparatively small, elastic modelling quantity
High.And noticeable be affected by irradiation after its elastic modelling quantity of material reduced, stress value increased (Fig. 1 (b)).
Meanwhile, the density of material increased (Fig. 2) after irradiation.Obviously material occurs in that after irradiation certain radiation aging is existing
As.
Use 3DSM and SEM method, the specimen surface after predose and stretching fracture are observed.Fig. 3 can see
Go out on the matrix of material, have the crackle not being fully disconnected, it is further seen that matrix on there is tiny flash of light striped, i.e.
Crazing.This is mainly made up of some height-oriented fibre bundles, and these fine crackles become the germination point that cracking is initial.
The generation of this phenomenon is to occur owing to irradiation creates tremendous influence to the surface of material.After Fig. 4 is predose
Stretching fracture microscopic appearance, it can be seen that section is the most smooth, and the fracture crack initiation point of sample occurs in surface rather than interior
Portion, has radial-like streak to emit (Fig. 4 (a)) from the starting point of crackle, belongs to the cleavage pattern of standard.After irradiation, sample
Cleavage surface on occur in that several obvious tongue crackles (Fig. 4 (c)).The formation mechenism of this tongue crackle be typically by
Be there is deviation thus produce in the forward position being made crackle by the separation of the plane between twin and matrix.Internal fragility district simultaneously
Territory increases, and illustrative material occurs certain brittle phenomenon after irradiation.
Have employed infrared spectrum (FTIR) and differential scanning calorimetry (DSC) further, to material surface and internal junction
Structure composition and situation of change are studied.FTIR detects 1300 cm-1The change at neighbouring peak.1305 cm-1With 1288 cm-1
At two, the relative intensity of absworption peak there occurs that change (Fig. 5), the degree of crystallinity after inferring predose accordingly there occurs change.DSC divides
Analysis shows, PEEK is after electron beam irradiation, and the hot property of material there occurs trickle change (Fig. 6), specifically, after irradiation
The fusing point of PEEK drops to 335 DEG C from 340 DEG C, and endothermic peak area is down to 30J/g from 38.5J/g, but glass transition temperature becomes
Change little, at 149 ~ 152 DEG C.May infer that the intensification along with irradiation dose, the crystal structure of material is no longer as the most steady
Determining, and degree of crystallinity has declined, crystal region is formed after being destroyed again has defective small crystalline structure.Meanwhile,
If the carefully DSC image after contrast predose, it can be seen that the melt initiation temperature degree of material PEEK is with the increasing of accumulation irradiation dose
Add and reduce, and irradiation postpeak type broadens, poor compared with before material irradiation of the crystallization regularity after this explanation irradiation.In conjunction with
FTIR analysis result can be determined that the degree of crystallinity of material decreases under the conditions of irradiation dose.
Then Raman spectrum is utilized to observe carbon backbone structure situation of change, as shown in Figure 7.After contrast predose, sample draws
Graceful spectrum, it is found that the scattering peak intensity increase of saturated C-H after irradiation, illustrates that in irradiation process, PEEK strand is handed over
Connection, intramolecular unsaturated group ratio reduces.Analysis before Zong He understands, and crystallization regularity is mainly determined by the degree of cross linking
Fixed, because the increase of cross-linked structure causes material crystalline degree to reduce.The rising of glass transition temperature demonstrates segmental mobility and becomes
Difference, also illustrates the generation of cross-linking reaction when high dosage irradiation, and in material noncrystalline domain, the increase of cross-linked structure hinders crystalline substance
The Relative sliding in district, becomes fragile so result in material, and in drawing process, elongation at break reduces.
From this it can be concluded that the radiation aging damage reason of polyether-ether-ketone is predominantly handed under the conditions of this irradiation dose
Connection reconstruct.
Embodiment 2: the Aging Damage reason under the conditions of radiation dose rate and analysis
Fig. 8 show the stretching force value deformation curve before and after gamma-ray irradiation close rate condition.Can be seen that polyether-ether-ketone material
Expecting that the elongation at break after predose under this condition decreases, there is certain Aging Damage in material mechanical performance.
The microscopic appearance of Tensile fracture is observed further with SEM.It is observed that material internal is divided into Liang Ge district equally
, all there is semicircular face of dissociating in territory at lower edges, crackle extends inward from surface；At right half part short texture,
Surface irregularity, for toughness district (Fig. 9 (a)).Stretching lines in cleavage surface turns white because of stress, can be seen that it after amplification
Deformation pattern (Fig. 9 (b), (c)), this is that polymer occurs in that microcrack body, countless microcrack body collection under tensile stress effect
In together, owing to the density from material is different, index of refraction is different, so seeming and turning white, have ligule decorative pattern to occur simultaneously.Thus
May determine that, the tension failure form of the material under the conditions of different radiation dose rates is essentially identical with predose, belongs to dissociative type
Fracture.
Use FTIR and DSC that the polyether-ether-ketone under the conditions of Different Dose Rates is studied again.FTIR atlas analysis shows,
When low dose rate, at 1740 cm-1With 1723 cm-1Place occurs in that new absworption peak, and illustrative material is because of energetic gamma rays irradiation
Cause molecular scission to form free radical (Figure 10), so react with oxygen produce new containing carbonyl material；Meanwhile,
1305 cm-1With 1288 cm-1Place's absworption peak is it is found that along with the increase of radiation dose rate, the intensity of the former with the latter is relative
Ratio decreases, it means that the decline of material crystalline degree.DSC studies display, under the conditions of irradiation accumulated dose, along with irradiation agent
The rising of dose rate, the glass transition temperature of material is significantly raised, reaches 6 DEG C compared to predose amplification during 10kGy/h；And melt
Enthalpy has then raised when low dose rate (0.5kGy/h), declines when high dose rate (10kGy/h), and difference therebetween reaches
10J/g, there is competitive relation in this phenomenon explanation test material oxidative degradation and cross-linking reaction degree when low dose rate；And it is interior
The cross-linked network ratio in portion increases when high-dose-rate irradiation so that the strand activeness of material is obstructed, aging the tightest
Weight.
From this it can be concluded that there is oxidative degradation and cross-linking reaction under this close rate radiation parameter simultaneously, and high agent
During dose rate gamma-ray irradiation, cross-linking reaction accounts for leading.
Embodiment 3: the Aging Damage reason under irradiation temperature and analysis
Figure 11 shows that the polyether-ether-ketone after room temperature predose and 80 DEG C of gamma-ray irradiations stretches force value deformation curve figure.Contrast can
To find out, tensile strength and elongation at break change after material predose under this condition are little, and material mechanical performance is aging
Degree is inconspicuous.
Then SEM is utilized to observe the stretching fracture pattern under this radiation parameter, as shown in figure 12.It can be seen that
Tension failure original position after this radiation parameter is equally at specimen surface, and breaking part is semicircle shape cleavage surface, and on it, existence is put
Penetrate shape crackle (Figure 12 (b)), belong to cleavage fracture feature；Fracture edges also has flexural deformation vestige (Figure 12 (c)), illustrative material
Now there is certain toughness.Preliminary it can be assumed that material fracture mode under this condition is dissociative type, irradiation damage degree
The highest.
Figure 13 demonstrates FTIR spectrum analysis result, and after contrast predose, infrared spectrogram understands, at 1306 cm-1With
1278 cm-1The strong ratio of characteristic peak at place changes along with the rising of irradiation temperature not quite, illustrates material crystalline under hot conditions
The change of degree is less.Additionally, at 1700 cm-1Place's the most significantly oxidation carbonyl peak occurs, the oxidation of material under the conditions of this is described
Degree is the highest.After 80 DEG C of gamma-ray irradiations, the DSC result of sample shows, slightly raises relative to predose Tg and Tm, and Tm protects
Hold at about 339 DEG C (Figure 14).
From this it can be concluded that the Aging Damage degree of polyether-ether-ketone is relatively low under this radiation parameter, the resistance to 80 DEG C of γ of material
Irradiation ability is stronger.
Claims (4)
1. the nuclear power synthetic judgement of engineering plastics radiation aging damage reason, it is characterised in that described nuclear power recruitment
Engineering plastics is polyetheretherketonematerials materials, specifically comprises the following steps that
Step one: detect the physical and mechanical property of the polyetheretherketonematerials materials after x ray irradiation x, analyzes it at different irradiation
The situation of change of physical and mechanical property before and after condition process, the situation of change of described physical and mechanical property includes: density of material is
No change, whether the tensile strength of material degenerates；
Step 2: outward appearance and the stretching fracture microscopic appearance to the polyetheretherketonematerials materials after x ray irradiation x, uses said three-dimensional body formula to show
Micro mirror (3DSM) and scanning electron microscope (SEM) are observed, and the physical and mechanical property test result of integrating step one, to spoke
Polyetheretherketonematerials materials tension failure form after according to carries out preliminary judgement；Tension failure pattern is divided into 3 kinds: ductile rupture, general
Brittle fracture and dissociative type fracture；
Step 3: on the basis of step 2 tentatively judges, uses infrared spectrum (FTIR) or thermal performance analysis further
(DSC) one or more in detection means, to inside and outside polyetheretherketonematerials materials after predose, stretching fracture position carry out microcosmic table
Levy analysis and test, so that it is determined that polyetheretherketonematerials materials situation of change of degree of crystallinity in irradiation process；
Step 4: on the basis of step 3, recycling infrared spectrum (FTIR), Raman spectrum (Raman), scanning electron microscope
(SEM) and energy spectrum analysis (EDS) detection means, integrating step two and the analysis result of step 3, determine that polyether-ether-ketone is irradiated
Aging Damage reason in journey；The reason causing Aging Damage is broadly divided into 2 kinds: oxidation reaction and crosslinking reconstruct.
Decision method the most according to claim 1, it is characterised in that in step 2:
3DSM and SEM is used to observe overall pattern and the stretching fracture microscopic appearance of polyetheretherketonematerials materials after predose, by difference
Observed result under radiation parameter contrasts, it is judged that the fracture mode belonging to polyetheretherketonematerials materials；
If the feature of stretching fracture is: Tensile fracture is uneven, short texture, there is the structures such as circular dimple, edge with
Corrugated lines；Then fracture mode is ductile rupture；
If the feature of stretching fracture is: Tensile fracture is concordant, compact structure, micro-crack or radial crack occur；Then rupture mould
Formula is general brittle fracture；
If the feature of stretching fracture is: exist circular or semicircular smooth concordant, it exists strip cracking lines, and split
Stricture of vagina propagation direction is consistent, can be also found that tongue pattern form crackle simultaneously；Then fracture mode is dissociative type fracture.
Decision method the most according to claim 1, it is characterised in that in step 3:
Microscopic sdIBM-2+2q.p.approach analysis is carried out for the polyetheretherketonematerials materials after predose, uses FTIR spectrum to analyze its microstructure, if
1305 cm-1(the bending vibration peak of agraphitic carbon skeleton) and 1288 cm-1The intensity at (the antisymmetric stretching vibration peak of diphenyl ether)
Ratio raises；Use DSC that hot property is analyzed simultaneously, find that inner molten enthalpy declines, it is determined that its Aging Damage causes
The degree of crystallinity of polyetheretherketonematerials materials reduces；Otherwise, then crystal region change is little.
Decision method the most according to claim 3, it is characterised in that in step 4:
For step 3 determines the polyetheretherketonematerials materials that degree of crystallinity reduces, FTIR and Raman is used to analyze its characteristic group
And carbon backbone structure, use SEM to observe its microscopic appearance；If collection of illustrative plates finds oxide group characteristic peak, microscopic appearance occurs
The results such as pore, it is determined that its Aging Damage reason is oxidation reaction；
For determining the polyetheretherketonematerials materials that degree of crystallinity reduces in step 3, if finding in collection of illustrative plates, molecular carbon framing structure changes,
Oxide group characteristic peak is without new change；In microscopic appearance, brittle zone ratio increases, without notable air hole structure, it is determined that it is old
Change damage reason for crosslinking reconstruct.
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| CN107490526A (en) * | 2017-09-06 | 2017-12-19 | 中国工程物理研究院核物理与化学研究所 | Macromolecule material aging effect the cannot-harm-detection device and its detection method |
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