CN102507370B - Method for measuring density of microsphere and surface coating thereof - Google Patents
Method for measuring density of microsphere and surface coating thereof Download PDFInfo
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- CN102507370B CN102507370B CN 201110318993 CN201110318993A CN102507370B CN 102507370 B CN102507370 B CN 102507370B CN 201110318993 CN201110318993 CN 201110318993 CN 201110318993 A CN201110318993 A CN 201110318993A CN 102507370 B CN102507370 B CN 102507370B
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Abstract
The invention discloses a method for measuring the density of microspheres and surface coating thereof, belonging to the technical field of microsphere measurement. The method comprises the following steps: B, pouring the microspheres to be measured into a sample introduction tank, and recording the number of the microspheres to be measured; C, making the microspheres to be measured enter a falling device from the sample introduction tank, and collecting the dynamic images of the falling microspheres to be measured; D, sieving the images of the microspheres to be measured; E, calculating the mass of the single microsphere to be measured according to the total mass and number of the microspheres to be measured, and calculating the volume of the single microsphere to be measured according to the sieved images of the microspheres to be measured; F, coating the surfaces of the microspheres to be measured to obtain coated microspheres, and subjecting the coated microspheres to operation from the step B to the step E repeatedly to obtain the mass and the volume of the coated microspheres; and G, calculating the density of the microspheres and the surface coating thereof. The method is easy to operate with less people involved and can be used for rapidly and precisely measuring the density of the microspheres and the surface coating thereof without causing pollution.
Description
Technical field
The present invention relates to the microballoon field of measuring technique, particularly the measuring method of a kind of microballoon and surface coating density thereof.
Background technology
Density is one of important indicator of material physical property, and for the microballoon that has surface coating, microballoon density and surface coating density thereof directly influence its character and application.
The employed spheric fuel element structure of China's ball bed high temperature gas cooled reactor is that spherical coated particle (TRISO) disperse is in the graphite matrix of fuel region.The nuclear core of coated particle is UO
2Ceramic microsphere is at UO
2Three layers of pyrolytic carbon of heat deposition (PyC) layer and one deck silicon carbide layer, wherein UO on the nuclear core
2The major function of nuclear core is: 1. nuclear fission takes place produce nuclear energy; 2. be detained a part of radioactive fission product.The major function of loose pyrolytic carbon layer: 1. porous is gas fission product, CO and CO
2The storage area is provided, has reduced the internal pressure of coated particle; 2. cushion by the nuclear fission generation and from the nuclear fission fragment that the fuel kernel wicking surface flies out, fine and close pyrolytic carbon layer sustains damage in preventing; 3. absorb the swelling of the fuel kernel core that causes because of burnup.Coated particle is the key components of high temperature nuclear reactor fuel element, and in fact each coated particle is exactly a miniature fuel element.Must strict control UO in fuel element is produced
2Thickness, the density of the loose pyrolytic carbon layer of diameter, density and the coated particle of nuclear core.The method of measuring the loose pyrolytic carbon layer density of coated particle at present comprises X-ray-projection amplifying method, single ball quality-size method, mercury intrusion method etc.
1, X-ray-projection amplifying method
This method is that Tsing-Hua University's nuclear grinds institute at the high temperature gas-cooled experimental reactor UO of research 10MW
2Grow up during the measuring method of nuclear core diameter and coating thickness, the difference that it absorbs X-ray according to the material of different densities, utilize trickle ball egative film to carry out 1: 1 radiograph to coating microballoon, then egative film is carried out the measurement one by one of coating thickness and nuclear core diameter at the optical grating projection instrument, obtain average external volume and the single UO of single ball weaker zone thus
2The average external volume of nuclear core is again according to the UO that measures in addition
2Nuclear core density calculates weaker zone density.The problem that this method exists is to introduce more human factor, and efficient is low, and the surveying work amount is big, is difficult to realize online quick measurement.
2, single ball quality-size method
Generally speaking, single ball quality-size method is taken out the microsphere particle of 10 coatings at random to every batch sample, place the quality of the microsphere particle that weighs up single coating in the monkey respectively, carrying out material object then under the optical grating projection instrument measures, measure the diameter of microsphere particle on 6 different directions of single coating, record data, then the surface coating of each coating microsphere particle is got rid of, weighing is also measured diameter on 6 different directions of corresponding microballoon, calculates the density of 10 microsphere particle surface coatings respectively.The shortcoming of this method is, because the restriction of method itself, sampling number is few, and under the unsettled situation of cladding process, the loose charcoal layer density variation that 10 microballoons are surveyed is bigger.
3, mercury intrusion method
Adopt the mercury injection apparatus test to coat the volume of microballoon, this method can increase substantially test speed, the specimen wide ranges, sample shape there is not specific (special) requirements, and sampling number is big, and is representative, but its operating conditions harshness, the processing of radioactive sample and mercury, recovery difficulty pollute easily.
Summary of the invention
(1) technical matters that will solve
The technical problem to be solved in the present invention is: how the measuring method of a kind of microballoon and surface coating density thereof is provided so as fast, high precision, free of contamination measurement microballoon and surface coating density thereof.
(2) technical scheme
For solving the problems of the technologies described above, the invention provides the measuring method of a kind of microballoon and surface coating density thereof, it comprises step:
B: pour microballoon to be measured into the sample introduction groove, when described microballoon to be measured rolls, record the quantity of described microballoon to be measured in described sample introduction groove;
C: described microballoon to be measured enters falling apparatus from described sample introduction groove, and the microballoon described to be measured that is in the dropping process is carried out dynamic image acquisition;
D: the image to described microballoon to be measured screens, and obtains screening the image of back microballoon to be measured;
E: according to the quality that gross mass and the quantity of described microballoon to be measured obtains single microballoon to be measured, obtain the volume of single microballoon to be measured according to the image calculation of screening back microballoon to be measured;
F: after the surface of described microballoon to be measured arranged coating, obtain coating microballoon, described coating microballoon is repeated described step B to E, obtain quality and the volume of single coating microballoon;
G: according to quality and the volume of single microballoon to be measured, and the quality of single coating microballoon and volume, calculate the density of described microballoon to be measured and coating.
Preferably, before described step B, also comprise steps A: the gross mass that makes the described microballoon to be measured that weighs with scale.
Preferably, among the described step B, described feed well is arranged rolling with the predetermined vibration frequency vibration so that described microballoon to be measured is single formation.
Preferably, among the described step C, adopt laser detection system according to predetermined filming frequency described microballoon to be measured to be carried out dynamic image acquisition.
Preferably, described predetermined filming frequency is between 10 to 450Hz.
Preferably, described step D specifically comprises step:
D1: according to the standard value of maximum gauge, minimum diameter, circularity, length breadth ratio and the mean diameter of described microballoon to be measured, adopt computing machine that the image of described microballoon to be measured is screened, deletion dust image reaches the image of the microballoon to be measured that is not single disperse state;
D2: browse the image of the microballoon to be measured after the screening, judge whether the image of the microballoon to be measured that remains the dust image and be not single disperse state, if having, carry out described step D1, otherwise, carry out described step e.
Preferably, described step e specifically comprises step:
E1: the quality that obtains single microballoon to be measured according to gross mass and the quantity of described microballoon to be measured;
E2: according to the image of screening back microballoon to be measured, obtain screening mean diameter, maximum gauge, minimum diameter and the standard deviation of each microballoon to be measured in the microballoon to be measured of back, and then calculate the mean diameter of screening back microballoon to be measured, as the mean diameter of all microballoons to be measured;
E3: according to the mean diameter of described all microballoons to be measured, calculate the volume of single microballoon to be measured.
Preferably, described step G specifically comprises step:
G1: the density that calculates described microballoon to be measured according to quality and the volume of single microballoon to be measured;
G2: according to the quality of single microballoon to be measured and the quality of single coating microballoon, calculate the quality of described coating;
G3: according to the volume of single microballoon to be measured and the volume of single coating microballoon, calculate the volume of described coating;
G4: according to quality and the volume of described coating, calculate the density of described coating.
Preferably, described microballoon to be measured comprises: the spherical object of paddy, mineral, metal, pottery, glass and uranium dioxide material; Described coating adopts metal material or Inorganic Non-metallic Materials.
Preferably, the numerical range of described microballoon to be measured and coating diameter of micro ball is from 10 to 10000 microns.
(3) beneficial effect
The measuring method of microballoon of the present invention and surface coating density thereof, record the quantity of microballoon to be measured and coating microballoon by photoelectric counter, multi-angle image according to microballoon to be measured and coating microballoon calculates its volume, simple to operate, artificial participate in few, can be fast, high precision, free of contamination measurement microballoon and surface coating density thereof.And because microballoon sample size to be measured is big, the multi-angle image for the treatment of micrometer ball and coating microballoon screens, and has further improved the precision of measurement result.
Description of drawings
Fig. 1 is the measuring method process flow diagram of the described microballoon of the embodiment of the invention and surface coating density thereof.
Embodiment
Below in conjunction with drawings and Examples, the specific embodiment of the present invention is described in further detail.Following examples are used for explanation the present invention, but are not used for limiting the scope of the invention.
Fig. 1 is the measuring method process flow diagram of the described microballoon of the embodiment of the invention and surface coating density thereof.As shown in Figure 1, described method comprises:
Steps A: use the gross mass of a certain amount of microballoon to be measured of the accurate weighing of electronic balance, and record this gross mass value.
Step B: pour described microballoon to be measured into the sample introduction groove, when described microballoon to be measured rolls in described sample introduction groove, adopt photoelectric counter to record the quantity of described microballoon to be measured.Here should note pouring described microballoon to be measured into described sample introduction groove with moderate ground speed, described sample introduction groove is simultaneously with the predetermined vibration frequency vibration, be listed in to roll in the described sample introduction groove and advance thereby make described microballoon to be measured be single queue, described photoelectric counter easy to use records the quantity of described microballoon to be measured.
Step C: described microballoon to be measured enters falling apparatus from described sample introduction groove end, adopts laser detection system, to being in the microballoon described to be measured in the dropping process, carries out dynamic image acquisition according to predetermined filming frequency.The predetermined filming frequency here generally between 10 to 450Hz, in described microballoon dropping process to be measured, can carry out repeatedly (such as 20 times) to each microballoon to be measured and take, thereby obtains the image of the different angles of each microballoon to be measured.Filming frequency is more high, and the granular information of each that obtains microballoon to be measured is more comprehensive.Described microballoon to be measured enters from the end of falling apparatus and connects the sample bag and be recovered, to be used for follow-up measurement.
Step D: the image to described microballoon to be measured screens, and obtains screening the image of back microballoon to be measured.Described step D further comprises:
Step D1: according to the standard value of maximum gauge, minimum diameter, circularity, length breadth ratio and the mean diameter of described microballoon to be measured, adopt computing machine that the image of described microballoon to be measured is screened, deletion dust image reaches the image of the microballoon to be measured that is not single disperse state.According to production specification, the maximum gauge of each described microballoon to be measured, minimum diameter, circularity, length breadth ratio and mean diameter should be floated near standard value among a small circle.Therefore, can set the isoparametric tolerance interval of maximum gauge, minimum diameter, circularity, length breadth ratio and mean diameter, utilize computing machine that the image that obviously departs from described standard value is carried out the preliminary screening deletion then, this part deleted image generally is dust image or the image that is not the microballoon to be measured of single disperse state (being the image that a plurality of microballoons to be measured connect together).
Step D2: browse the image of the microballoon to be measured after the preliminary screening, judge whether the image of the microballoon to be measured that remains the dust image and be not single disperse state, if having, carry out described step D1, otherwise, execution in step E.Because parameter arranges may be unreasonable, image through the microballoon to be measured after once screening still may be mixed with the image that the dust image reaches the microballoon to be measured that is not single disperse state, this step is judged by manually browsing, if the image of finding still to be mixed with the dust image in the image after the screening and not being the microballoon to be measured of single disperse state, then get back to step D1, reset maximum gauge, minimum diameter, circularity, behind the isoparametric tolerance interval of length breadth ratio and mean diameter, image after the screening is screened again, so circulation, meet the requirements until image, thereby guarantee that effectively follow-up image for the microballoon to be measured that calculates is accurately and effectively.
Step e: according to the quality that gross mass and the quantity of described microballoon to be measured obtains single microballoon to be measured, obtain the volume of single microballoon to be measured according to the image calculation of screening back microballoon to be measured.
Described step e specifically comprises:
Step e 1: the quality that obtains single microballoon to be measured according to gross mass and the quantity of described microballoon to be measured.The gross mass of described microballoon to be measured obtains by electronic balance weighing, and quantity obtains by photoelectric counter, therefore, removes in its quantity with the gross mass of described microballoon to be measured, obtains the quality of single microballoon to be measured easily.
Step e 2: according to the image of screening back microballoon to be measured, obtain screening mean diameter, maximum gauge, minimum diameter and the standard deviation of each microballoon to be measured in the microballoon to be measured of back, and then calculate the mean diameter of screening back microballoon to be measured, as the mean diameter of all microballoons to be measured.Here need to prove, each microballoon to be measured self has a mean diameter value (being designated as first mean diameter), screening back microballoon to be measured totally has a mean diameter value (being designated as second mean diameter), and all microballoons to be measured totally have a mean diameter value (being designated as the 3rd mean diameter).The calculating principle here is: according to the image of screening back microballoon to be measured, obtain correlation parameters such as first mean diameter and maximum gauge, minimum diameter and standard deviation, and then calculate second mean diameter, and with described second mean diameter as described the 3rd mean diameter.
Step e 3: according to the mean diameter of described all microballoons to be measured, calculate the volume of single microballoon to be measured.
Step F: after the surface of described microballoon to be measured arranged coating, obtain coating microballoon, described coating microballoon is repeated described steps A to E, obtain quality and the volume of single coating microballoon.To through described microballoon described to be measured after connecing the sample bag and reclaiming, be coated with coating on the surface by methods such as physics coating or chemogenic deposits respectively, obtain coating microballoon, after replacing described microballoon to be measured with described coating microballoon then, repeat described steps A to E, obtain quality and the volume of single coating microballoon.Here, before described coating microballoon was carried out described step B to E, those skilled in the art expected easily, also should carry out described steps A to described coating microballoon, even with the gross mass of the described coating microballoon of electronic balance weighing, do not repeat them here.
Step G: according to quality and the volume of single microballoon to be measured, and the quality of single coating microballoon and volume, calculate the density of described microballoon to be measured and coating.
Described step G specifically comprises:
Step G1: the density that calculates described microballoon to be measured according to quality and the volume of single microballoon to be measured.
Step G2: utilize the quality of single coating microballoon to deduct the quality of single microballoon to be measured, calculate the quality of described coating.
Step G3: utilize the volume of single coating microballoon to deduct the volume of single microballoon to be measured, calculate the volume of described coating.
Step G4: utilize the quality of described coating except in its volume, calculate the density of described coating.
The described method of the embodiment of the invention can also be applied to the microballoon of materials such as paddy, mineral, metal, pottery, glass and the density measure of surface coating thereof except the density measure that can be applied to uranium dioxide microballoon and surface coating thereof.The numerical range of described microballoon and coating diameter of micro ball is from 10 to 10000 microns, and described coating can adopt metal material or Inorganic Non-metallic Materials.
The measuring method of the described microballoon of the embodiment of the invention and surface coating density thereof, record the quantity of microballoon to be measured and coating microballoon by photoelectric counter, multi-angle image according to microballoon to be measured and coating microballoon calculates its volume, simple to operate, artificial participate in few, can be fast, high precision, free of contamination measurement microballoon and surface coating density thereof.And because microballoon sample size to be measured is big, the multi-angle image for the treatment of micrometer ball and coating microballoon screens, and has further improved the precision of measurement result.
Above embodiment only is used for explanation the present invention; and be not limitation of the present invention; the those of ordinary skill in relevant technologies field; under the situation that does not break away from the spirit and scope of the present invention; can also make a variety of changes and modification; therefore all technical schemes that are equal to also belong to category of the present invention, and scope of patent protection of the present invention should be defined by the claims.
Claims (8)
1. the measuring method of a microballoon and surface coating density thereof is characterized in that, comprises step:
B: pour microballoon to be measured into the sample introduction groove, when described microballoon to be measured rolls, record the quantity of described microballoon to be measured in described sample introduction groove;
C: described microballoon to be measured enters falling apparatus from described sample introduction groove, and the microballoon described to be measured that is in the dropping process is carried out dynamic image acquisition;
D: the image to described microballoon to be measured screens, and obtains screening the image of back microballoon to be measured;
E: according to the quality that gross mass and the quantity of described microballoon to be measured obtains single microballoon to be measured, obtain the volume of single microballoon to be measured according to the image calculation of screening back microballoon to be measured;
F: after the surface of described microballoon to be measured arranged coating, obtain coating microballoon, described coating microballoon is repeated described step B to E, obtain quality and the volume of single coating microballoon;
G: according to quality and the volume of single microballoon to be measured, and the quality of single coating microballoon and volume, calculate the density of described microballoon to be measured and coating;
Wherein, among the step C, described microballoon to be measured enters from the end of falling apparatus and connects the sample bag and be recovered;
In the step F, described microballoon to be measured is the microballoon described to be measured that connects after the sample bag reclaims through described;
Described step D specifically comprises step:
D1: according to the standard value of maximum gauge, minimum diameter, circularity, length breadth ratio and the mean diameter of described microballoon to be measured, adopt computing machine that the image of described microballoon to be measured is screened, deletion dust image reaches the image of the microballoon to be measured that is not single disperse state;
D2: browse the image of the microballoon to be measured after the screening, judge whether the image of the microballoon to be measured that remains the dust image and be not single disperse state, if having, carry out described step D1, otherwise, carry out described step e;
The numerical range of described microballoon to be measured and coating diameter of micro ball is from 10 to 10000 microns.
2. the method for claim 1 is characterized in that, also comprises steps A before described step B: the gross mass that makes the described microballoon to be measured that weighs with scale.
3. the method for claim 1 is characterized in that, among the described step B, described feed well is arranged rolling with the predetermined vibration frequency vibration so that described microballoon to be measured is single formation.
4. the method for claim 1 is characterized in that, among the described step C, adopts laser detection system according to predetermined filming frequency described microballoon to be measured to be carried out dynamic image acquisition.
5. method as claimed in claim 4 is characterized in that, described predetermined filming frequency is between 10 to 450Hz.
6. the method for claim 1 is characterized in that, described step e specifically comprises step:
E1: the quality that obtains single microballoon to be measured according to gross mass and the quantity of described microballoon to be measured;
E2: according to the image of screening back microballoon to be measured, obtain screening mean diameter, maximum gauge, minimum diameter and the standard deviation of each microballoon to be measured in the microballoon to be measured of back, and then calculate the mean diameter of screening back microballoon to be measured, as the mean diameter of all microballoons to be measured;
E3: according to the mean diameter of described all microballoons to be measured, calculate the volume of single microballoon to be measured.
7. the method for claim 1 is characterized in that, described step G specifically comprises step:
G1: the density that calculates described microballoon to be measured according to quality and the volume of single microballoon to be measured;
G2: according to the quality of single microballoon to be measured and the quality of single coating microballoon, calculate the quality of described coating;
G3: according to the volume of single microballoon to be measured and the volume of single coating microballoon, calculate the volume of described coating;
G4: according to quality and the volume of described coating, calculate the density of described coating.
8. as the described method of one of claim 1 to 7, it is characterized in that described microballoon to be measured comprises: the spherical object of paddy, mineral, metal, pottery, glass and uranium dioxide material; Described coating adopts metal material or Inorganic Non-metallic Materials.
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| CN107870056B (en) * | 2017-11-09 | 2019-12-13 | 中国工程物理研究院激光聚变研究中心 | Device and method for measuring pressure intensity of gas in microsphere |
| CN108007819A (en) * | 2017-11-29 | 2018-05-08 | 合肥赑歌数据科技有限公司 | A kind of hollow steel ball qualification analysis system and method based on discrete analysis |
| CN110044769B (en) * | 2019-05-06 | 2022-03-11 | 中建材蚌埠玻璃工业设计研究院有限公司 | Method for measuring specific gravity of hollow glass beads |
| CN112362529A (en) * | 2020-11-03 | 2021-02-12 | 安徽省皖北煤电集团有限责任公司 | Soil volume weight determination method |
| EP4075117B1 (en) * | 2021-04-14 | 2024-05-01 | MTU Aero Engines AG | Method and device for characterizing a coating |
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| CN102564519A (en) * | 2011-11-23 | 2012-07-11 | 昆明理工大学 | Method for measuring and calculating volume and density of coating layer of complex coated workpiece and device |
| CN102680358A (en) * | 2012-05-31 | 2012-09-19 | 清华大学 | Method for measuring densities of porous coatings on surfaces of fuel particles |
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