CN107543819A - MOX pellet metallographic detection methods - Google Patents
MOX pellet metallographic detection methods Download PDFInfo
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- CN107543819A CN107543819A CN201710753185.7A CN201710753185A CN107543819A CN 107543819 A CN107543819 A CN 107543819A CN 201710753185 A CN201710753185 A CN 201710753185A CN 107543819 A CN107543819 A CN 107543819A
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Abstract
The invention belongs to product analysis detection technique field, and in particular to a kind of MOX pellets metallographic detection method.From the mox fuel pellet of the complete flawless in surface；Vulcanized sodium, configuration edge sample agent are added into epoxy resin；Mox fuel pellet is placed on to the center of phenolic resin edge sample set, pours into edge sample agent, is stood after edge sample agent solidification, the sample inlayed is taken out from edge sample set；The sample inlayed is attached in grinding and polishing equipment chuck and fixed, is ground respectively on grinding and polishing disk from coarse to fine, rinses sample with water when changing grinding and polishing disk every time；Cleaned sample is continued to be arranged in chuck and fixed, sample is polished on flannelette, while Al2O3 liquid for polishing is poured on grinding and polishing disk, grinding and polishing with water rinses sample after terminating；According to sample quantities, etch is carried out to sample after polishing with HNO3 and HCl configuration corrosive liquids, stops rinsing specimen surface with water after corroding, and rinsed and dried up with absolute ethyl alcohol.The accurate measurement of the achievable pellet crystallite dimension of the present invention and stomata equivalent diameter.
Description
Technical field
The invention belongs to product analysis detection technique field in nuclear fuel production process, and in particular to a kind of MOX pellets gold
Phase detection method.
Background technology
Crystallite dimension and stomata equivalent diameter are the critical technical parameters of mox fuel pellet, the compacting fast to cartridge and
The setting of sintering process parameter has directive significance, while pellet microstructure directly influences use of the pellet in reactor
Effect.At present, traditional fuel pellet metallographic e measurement technology is primarily present 4 points of deficiencies, first, mox fuel pellet structure is smaller
And containing center hole structure, conventional pressurized water heap pellet grinding and polishing handling process can cause MOX pellets cracking, crush；Second, mox fuel
Pellet containing uranium, plutonium element, therefore the corrosive agent of traditional pellet due to being not particularly suited for MOX pellet samples；Third, MOX pellets by
In the presence of pore creating material, traditional etching process is caused to cause the serious excessive erosion phenomenon of MOX pellets；Fourth, MOX pellet uranium plutoniums
Material radioactivity is strong, and traditional manual grinding and polishing can cause personnel excessively to be shone.
The content of the invention
It is an object of the invention to provide a kind of MOX pellets metallographic detection method, solve grinding and polishing efficiency is low, corrosive effect not
The problems such as obvious, realize pellet crystallite dimension and the accurate measurement of stomata equivalent diameter.
To reach above-mentioned purpose, the technical solution used in the present invention is：
A kind of MOX pellets metallographic detection method, comprises the following steps：
Step 1：From surface is complete, mox fuel pellet of flawless；
Step 2：Vulcanized sodium is added into epoxy resin, sample agent is inlayed according to metallographic analyzing specimen quantity configuration；
Step 3：Mox fuel pellet is placed on to the center of phenolic resin edge sample set, pours into edge sample agent, standing is treated
After inlaying sample agent solidification, the sample inlayed is taken out from edge sample set；
Step 4：1~6 sample inlayed is attached in grinding and polishing equipment chuck, sample fixed, respectively by thick
Grind on to thin grinding and polishing disk, rinse sample with H2O when changing grinding and polishing disk every time；
Step 5：Cleaned sample is continued to be arranged in chuck, sample is fixed, sample thrown on flannelette
Light, while Al2O3 liquid for polishing is poured on grinding and polishing disk, grinding and polishing with H2O rinse sample after terminating；
Step 6：According to sample quantities, with HNO3 and HCl configuration corrosive liquids, etch is carried out to sample after polishing, stopped rotten
Specimen surface is rinsed with H2O after erosion, and is rinsed and dried up with absolute ethyl alcohol；
Step 7：Metallographic microscope power supply is opened, sample is put on objective table, regulation microscope focus makes observed
As clear, regulation field stop makes sample be located at visual field center, and opening field stop makes its edge picture just disappear in outside visual field,
First carrying out after coarse adjustment further fine setting Jiao makes as clear, adjusts X on objective table, Y-axis turn-knob selects desired image, observe regarding
Whether it is to meet to require that microstructure is seen in, button of taking pictures such as is click on, if it is not, then continuing to choose visual field, directly
Taken pictures again to satisfactory image is obtained, shooting closes metallographic microscope after terminating, and sample is put into container and preserved.
Vulcanized sodium is added into epoxy resin according to 5~25% volume ratio in described step two, configures 20~100ml
Edge sample agent, 20-30ml is configured during 1 metallographic analyzing specimen.
5~10ml edge sample agent is poured into 1~5ml/min speed in described step three, stands 6~24h.
Sample is fixed from 5~30N pressure in described step four, with 10~200rpm speed respectively by
Slightly to 5~45min is ground on thin grinding and polishing disk, when changing grinding and polishing disk every time by sample with 0.2~3L/min H2O flushings 1~
10min。
Sample is fixed from 1~5N pressure in described step five, with 10~60rpm speed on flannelette it is right
Sample polishes 0.5~20min, while 10~50%w.t. Al2O3 liquid for polishing is poured with 10~100ml/min speed and ground
On dumping, grinding and polishing with 0.2~3L/min H2O rinses sample 1~5min after terminating.
In described step six with 30% volumetric concentration HNO3 and 1%-5% volumetric concentration HCl configuration corrosive liquid 20~
200ml, etch is carried out to sample after polishing, etching time 15min, is tried after stopping corrosion with 0.2~3L/min H2O flushings
1~5min of sample surface.
Having the beneficial effect that acquired by the present invention：
The present invention avoids pellet from ftractureing by using rational grinding and polishing process, and pellet crystal boundary is avoided from rational corrosive liquid
With stomatic observation unobvious, etching process is improved, prevents the generation of excessive erosion phenomenon, improves crystallite dimension and stomata equivalent diameter
The degree of accuracy of measurement.Verification experimental verification is detected through MOX pellets metallographic, equivalent direct six times of the crystallite dimension and stomata of MOX pellets are solely
Vertical measurement result relative standard deviation is less than 10%, can meet the precision requirement of MOX pellets Metallographic Analysis detection.In addition,
The present disclosure applies equally to the crystallite dimension of other fuel balls and stomata equivalent diameter to measure, treatment effect and reliability
Height, requirement of the nuclear fuel to metallography microscope structure observation can be met.
Embodiment
With reference to specific embodiment, the present invention is described in detail.
MOX pellets metallographic detection method of the present invention comprises the following steps：
Step 1：From surface is complete, mox fuel pellet of flawless.
Step 2：Vulcanized sodium is added into epoxy resin according to 5~25% volume ratio, according to metallographic analyzing specimen quantity
Configure 20~100ml edge sample agent.20-30ml is configured during 1 metallographic analyzing specimen.
Step 3：Mox fuel pellet is placed on to the center of phenolic resin edge sample set, with 1~5ml/min speed
5~10ml edge sample agent is poured into, 6~24h is stood after edge sample agent solidification, the sample inlayed is taken out from edge sample set.
Step 4：1~6 sample inlayed is attached in grinding and polishing equipment chuck, from 5~30N pressure by sample
Fix, 5~45min is ground on grinding and polishing disk from coarse to fine with 10~200rpm speed respectively, changes grinding and polishing disk every time
When sample rinsed into sample 1~10min with 0.2~3L/min H2O.
Step 5：Cleaned sample is continued to be arranged in chuck, fixed sample from 1~5N pressure, with
10~60rpm speed on flannelette to sample polish 0.5~20min, while by 10~50%w.t. Al2O3 liquid for polishing with
10~100ml/min speed is poured on grinding and polishing disk, and grinding and polishing with 0.2~3L/minH2O rinses sample 1~5min after terminating.
Step 6：According to sample quantities, corrosive liquid is configured with 30% volumetric concentration HNO3 and 1%-5% volumetric concentration HCl
20~200ml, etch is carried out to sample after polishing, etching time 15min, is stopped after corroding with 0.2~3L/min H2O water
1~5min of specimen surface is rinsed, and is rinsed and dried up with absolute ethyl alcohol.
Step 7：Metallographic microscope power supply is opened, sample is put on objective table, regulation microscope focus makes observed
As clear, regulation field stop makes sample be located at visual field center, and opening field stop makes its edge picture just disappear in outside visual field,
First carrying out after coarse adjustment further fine setting Jiao makes as clear, adjusts X on objective table, Y-axis turn-knob selects desired image, observe regarding
Whether it is to meet to require that microstructure is seen in, button of taking pictures such as is click on, if it is not, then continuing to choose visual field, directly
Taken pictures again to satisfactory image is obtained, shooting closes metallographic microscope after terminating, and sample is put into container and preserved.
Claims (6)
- A kind of 1. MOX pellets metallographic detection method, it is characterised in that：Comprise the following steps：Step 1：From surface is complete, mox fuel pellet of flawless；Step 2：Vulcanized sodium is added into epoxy resin, sample agent is inlayed according to metallographic analyzing specimen quantity configuration；Step 3：Mox fuel pellet is placed on to the center of phenolic resin edge sample set, edge sample agent is poured into, stands sample to be inlayed After agent solidification, the sample inlayed is taken out from edge sample set；Step 4：1~6 sample inlayed is attached in grinding and polishing equipment chuck, sample fixed, respectively from coarse to fine Grinding and polishing disk on grind, every time change grinding and polishing disk when sample is rinsed with H2O；Step 5：Cleaned sample is continued to be arranged in chuck, sample is fixed, sample polished on flannelette, together When Al2O3 liquid for polishing is poured on grinding and polishing disk, grinding and polishing terminate after with H2O rinse sample；Step 6：According to sample quantities, with HNO3 and HCl configuration corrosive liquids, etch is carried out to sample after polishing, after stopping corrosion Specimen surface is rinsed with H2O, and is rinsed and dried up with absolute ethyl alcohol；Step 7：Metallographic microscope power supply is opened, sample is put on objective table, regulation microscope focus makes observed picture clear Clear, regulation field stop makes sample be located at visual field center, and opening field stop makes its edge picture just disappear in outside visual field, advanced Further fine setting Jiao makes as clear after row coarse adjustment, and X, Y-axis turn-knob select desired image on regulation objective table, observe in visual field Whether it is to meet to require that microstructure is seen, is such as click on button of taking pictures, if it is not, then continuing to choose visual field, until obtaining Obtain satisfactory image to take pictures again, shooting closes metallographic microscope after terminating, and sample is put into container and preserved.
- 2. MOX pellets metallographic detection method according to claim 1, it is characterised in that：In described step two according to 5~ 25% volume ratio adds vulcanized sodium into epoxy resin, configures 20~100ml edge sample agent, matches somebody with somebody during 1 metallographic analyzing specimen Put 20-30ml.
- 3. MOX pellets metallographic detection method according to claim 1, it is characterised in that：In described step three with 1~ 5ml/min speed pours into 5~10ml edge sample agent, stands 6~24h.
- 4. MOX pellets metallographic detection method according to claim 1, it is characterised in that：In described step four from 5~ 30N pressure fixes sample, and 5~45min is ground on grinding and polishing disk from coarse to fine respectively with 10~200rpm speed, Sample is rinsed into 1~10min with 0.2~3L/min H2O when changing grinding and polishing disk every time.
- 5. MOX pellets metallographic detection method according to claim 1, it is characterised in that：In described step five from 1~ 5N pressure fixes sample, and 0.5~20min is polished to sample on flannelette with 10~60rpm speed, while by 10~ 50%w.t. Al2O3 liquid for polishing is poured on grinding and polishing disk with 10~100ml/min speed, grinding and polishing terminate after with 0.2~3L/ Min H2O rinse 1~5min of sample.
- 6. MOX pellets metallographic detection method according to claim 1, it is characterised in that：With 30% in described step six Volumetric concentration HNO3 and 1%-5% volumetric concentration HCl configures 20~200ml of corrosive liquid, and etch, corrosion are carried out to sample after polishing Time is 15min, stops rinsing 1~5min of specimen surface with 0.2~3L/min H2O after corroding.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108896339A (en) * | 2018-04-04 | 2018-11-27 | 江苏科泰检测技术服务有限公司 | The preparation method of metallographic specimen |
| CN114689397A (en) * | 2020-12-29 | 2022-07-01 | 中核北方核燃料元件有限公司 | Preparation method of cobalt core nickel coating metallographic sample |
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| CN104878389A (en) * | 2015-06-01 | 2015-09-02 | 金川集团股份有限公司 | Pure-nickel metallographic etchant and corroding method using same |
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2017
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| CN104181027A (en) * | 2014-08-22 | 2014-12-03 | 南京市产品质量监督检验院 | Method for preparing gold metallographic sample and displaying texture of sample |
| CN104878389A (en) * | 2015-06-01 | 2015-09-02 | 金川集团股份有限公司 | Pure-nickel metallographic etchant and corroding method using same |
| CN104911536A (en) * | 2015-06-25 | 2015-09-16 | 山东农业大学 | Surface-nanocrystallization low-temperature aluminizing treatment method for steel products |
| CN105928767A (en) * | 2016-04-18 | 2016-09-07 | 河北钢铁股份有限公司 | Preparation method of nickel steel-containing sample for EBSD analysis |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108896339A (en) * | 2018-04-04 | 2018-11-27 | 江苏科泰检测技术服务有限公司 | The preparation method of metallographic specimen |
| CN114689397A (en) * | 2020-12-29 | 2022-07-01 | 中核北方核燃料元件有限公司 | Preparation method of cobalt core nickel coating metallographic sample |
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Application publication date: 20180105 |