CN111583153B - Three-dimensional reconstruction method for micro-nano level structure of porous composite material - Google Patents
Three-dimensional reconstruction method for micro-nano level structure of porous composite material Download PDFInfo
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- CN111583153B CN111583153B CN202010392266.0A CN202010392266A CN111583153B CN 111583153 B CN111583153 B CN 111583153B CN 202010392266 A CN202010392266 A CN 202010392266A CN 111583153 B CN111583153 B CN 111583153B
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- 238000000034 method Methods 0.000 title claims abstract description 25
- 239000002131 composite material Substances 0.000 title claims abstract description 24
- 239000003822 epoxy resin Substances 0.000 claims abstract description 29
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 29
- 239000000463 material Substances 0.000 claims abstract description 21
- 239000011148 porous material Substances 0.000 claims abstract description 19
- 239000002086 nanomaterial Substances 0.000 claims abstract description 18
- 238000005498 polishing Methods 0.000 claims abstract description 13
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 12
- 238000010884 ion-beam technique Methods 0.000 claims abstract description 5
- 238000005520 cutting process Methods 0.000 claims abstract description 4
- 230000011218 segmentation Effects 0.000 claims abstract description 4
- 229920005989 resin Polymers 0.000 claims description 17
- 239000011347 resin Substances 0.000 claims description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 238000005507 spraying Methods 0.000 claims description 3
- 239000000523 sample Substances 0.000 description 19
- 230000000052 comparative effect Effects 0.000 description 7
- 238000010586 diagram Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 239000004925 Acrylic resin Substances 0.000 description 3
- 229920000178 Acrylic resin Polymers 0.000 description 3
- 238000009835 boiling Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005470 impregnation Methods 0.000 description 2
- 238000010603 microCT Methods 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 238000003705 background correction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005429 filling process Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 229910002119 nickel–yttria stabilized zirconia Inorganic materials 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000007517 polishing process Methods 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
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- G06T5/94—
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/2202—Preparing specimens therefor
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/225—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion
- G01N23/2251—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion using incident electron beams, e.g. scanning electron microscopy [SEM]
-
- G—PHYSICS
- G06—COMPUTING; CALCULATING OR COUNTING
- G06T—IMAGE DATA PROCESSING OR GENERATION, IN GENERAL
- G06T17/00—Three dimensional [3D] modelling, e.g. data description of 3D objects
-
- G—PHYSICS
- G06—COMPUTING; CALCULATING OR COUNTING
- G06T—IMAGE DATA PROCESSING OR GENERATION, IN GENERAL
- G06T7/00—Image analysis
- G06T7/10—Segmentation; Edge detection
- G06T7/11—Region-based segmentation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/07—Investigating materials by wave or particle radiation secondary emission
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/10—Different kinds of radiation or particles
- G01N2223/104—Different kinds of radiation or particles ions
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/40—Imaging
- G01N2223/401—Imaging image processing
-
- G—PHYSICS
- G06—COMPUTING; CALCULATING OR COUNTING
- G06T—IMAGE DATA PROCESSING OR GENERATION, IN GENERAL
- G06T2207/00—Indexing scheme for image analysis or image enhancement
- G06T2207/10—Image acquisition modality
- G06T2207/10056—Microscopic image
- G06T2207/10061—Microscopic image from scanning electron microscope
Abstract
The invention provides a three-dimensional reconstruction method for a micro-nano structure of a porous material, which comprises the following steps of: filling the pores of a sample to be tested by adopting a mixture containing epoxy resin and a curing agent under a vacuum condition; taking out a sample to be tested before the epoxy resin is completely cured, and directly polishing the cross section of the material by utilizing an ion beam polishing machine; observing and selecting a polished cross section area by using an electron microscope, alternately cutting and scanning a sample by using a focused ion beam-scanning electron microscope to obtain a continuous two-dimensional image flow, then carrying out alignment treatment on the two-dimensional image flow, carrying out shadow correction on an image, carrying out material area segmentation on the two-dimensional image according to a material contrast difference, and finally reconstructing a micro-nano three-dimensional structure of the porous composite material based on the segmented two-dimensional digitized image. By adopting the technical scheme of the invention, the accurate three-dimensional reconstruction of the micro-nano structure of the porous composite material is realized.
Description
Technical Field
The invention relates to the technical field of three-dimensional reconstruction, in particular to a three-dimensional reconstruction method for a micro-nano structure of a porous composite material.
Background
At present, two main technical methods are available for three-dimensional reconstruction of micro-nano structures of composite materials. One is a synchrotron micro-CT scanning system that uses an industrial X-ray generator or synchrotron as the X-ray generator to scan the composite material layer by layer. While modern micro-CT scanning systems can obtain digitized three-dimensional reconstruction data with a resolution of 5um and higher, the resolution is far from adequate for micro-nano scale microstructures. Another digital three-dimensional reconstruction scanning technique relies on a focused ion beam-scanning electron microscope (FIB-SEM) dual-beam technique, which can achieve a resolution of up to 3nm, but this method requires the help of complex image processing techniques to filter out interference caused by pore background in the electron microscope image when processing the microstructure of the porous material, so that the accuracy of three-dimensional reconstruction is greatly affected. Especially for porous composites, the disturbing effects caused by this pore background will be more severe, so this technique is limited to three-dimensional reconstruction of the micro-nano-scale structure of the densified material. In addition, the traditional method needs to adopt mechanical grinding, the original structure of the material is affected by external force in the process, the micro-nano scale porous material is mechanically damaged, and the processed material area cannot be restored. At present, the existing method can not realize accurate three-dimensional reconstruction of the micro-nano structure of the porous composite material temporarily.
Disclosure of Invention
Aiming at the technical problems, the invention discloses a three-dimensional reconstruction method for a micro-nano structure of a porous composite material, which can accurately reconstruct the micro-nano structure of various functional porous composite materials.
In this regard, the invention adopts the following technical scheme:
a three-dimensional reconstruction method for a porous composite micro-nano structure, comprising the steps of:
step S1, filling pores of a sample to be tested by adopting a mixture containing epoxy resin and a curing agent under a vacuum condition; wherein, the epoxy resin is cold-inlaid epoxy resin which can be used for vacuum impregnation, namely, the viscosity is lower; further, the ambient temperature is room temperature;
s2, before the epoxy resin is completely cured, taking out a sample to be tested from the incompletely cured resin, and directly polishing the section of the material by using an ion beam polishing machine; further, the curing temperature was room temperature.
And S3, observing and selecting a polished cross section area by using an electron microscope, alternately cutting and scanning a sample by adopting a focused ion beam-scanning electron microscope (FIB-SEM) double-beam technology to obtain a continuous two-dimensional image stream, then carrying out alignment treatment on the two-dimensional image stream, carrying out shadow correction on an image, carrying out material area segmentation on the two-dimensional image according to the material contrast difference, and finally reconstructing a micro-nano three-dimensional structure of the porous composite material based on the segmented two-dimensional digital image.
According to the technical scheme, epoxy resin enters a composite material micro-nano structure to be filled under vacuum, and then a high-power ion beam polishing instrument is used for polishing the surface of a required sample, so that the conventional mechanical polishing step of a cured resin block is omitted, meanwhile, the damage in the mechanical polishing process is avoided, and the gap caused by the tearing of the boundary between the resin and a solid material is prevented; finally, the sample is alternately cut and scanned by a focused ion beam-scanning electron microscope (FIB-SEM) double-beam technology, and the scanned image can be displayed because the epoxy resin and the composite material are different in material, so that three-dimensional reconstruction is realized.
As a further improvement of the present invention, in step S1, the sample to be measured is immersed in a mixture containing an epoxy resin and a curing agent for pore filling, or the mixture containing an epoxy resin and a curing agent is used for pore filling by flowing over the surface of the sample to be measured.
As a further improvement of the invention, when the mixture of the epoxy resin and the curing agent flows through the surface of the sample to be tested for pore filling, the flow rate of the mixture of the epoxy resin and the curing agent is not more than 0.25mm/s.
As a further improvement of the present invention, in step S1, the vacuum degree is 0.1 to 0.15 atm. The vacuum level needs to be strictly controlled, and too high a pressure can lead to incomplete filling, and too low a pressure can lead to resin boiling and also to air bubbles.
As a further improvement of the present invention, step S1 further comprises allowing the filled sample to be measured to stand for 2 hours under an atmosphere of 0.1 to 0.15atm, and then curing.
As a further improvement of the present invention, in step S1, the epoxy resin is EpoFix Kit cold-set epoxy resin.
As a further improvement of the invention, in the step S2, the epoxy resin is firstly cured for 1-3 hours at room temperature, and when the hardness of the epoxy resin reaches 15-25% of the hardness of the epoxy resin which is completely cured, a sample is taken out of the resin which is not completely cured, and the curing is continued.
As a further improvement of the present invention, after finishing the polishing in step S2, the surface of the sample to be tested is subjected to carbon spraying treatment.
Compared with the prior art, the invention has the beneficial effects that:
by adopting the technical scheme of the invention, the cost of three-dimensional reconstruction of the micro-nano structure of the material is greatly reduced, and the background image in the hole is perfectly converted into a black background with zero contrast under the observation of an electron microscope by selecting proper resin and a filling process method. Meanwhile, the invention avoids the mechanical damage of the traditional mechanical grinding process to the micro-nano scale porous material, furthest keeps the original structure of the material from being influenced by external force, realizes the accurate three-dimensional reconstruction of the micro-nano scale structure of the porous composite material, and provides an accurate digital model for the quantitative research of the micro-nano scale structure of the material.
Drawings
FIG. 1 is a schematic diagram of a two-dimensional graphics stream obtained in example 1 of the present invention.
Fig. 2 is a three-dimensional creation chart obtained in embodiment 1 of the present invention.
FIG. 3 is a three-dimensional reconstruction after treatment obtained in example 1 of the present invention.
FIG. 4 is a partial schematic view of a three-dimensional reconstruction after processing obtained in example 1 of the present invention.
FIG. 5 is a partial schematic view of the three-dimensional reconstruction after treatment obtained in comparative example 1 of the present invention.
FIG. 6 is a partial schematic representation of the processed three-dimensional reconstruction obtained in comparative example 2 of the present invention.
Detailed Description
Preferred embodiments of the present invention are described in further detail below.
Example 1
A three-dimensional reconstruction method for a porous composite material micro-nano structure aims at three-dimensional reconstruction of a nickel-yttria stabilized zirconia metal-ceramic composite material and comprises the following steps:
(1) Slowly flowing the mixture of the low-viscosity epoxy resin and the curing agent through the surface of the sample at a speed of below 0.25mm/s under the vacuum condition at room temperature to fill the pores of the sample material; wherein the atmospheric pressure of the vacuum condition is 0.1-0.15atm, too low a vacuum (> 0.15 atm) results in incomplete filling, while too high a vacuum (< 0.1 atm) results in boiling of the resin, and also the introduction of bubbles. After filling, the sample was allowed to stand under an atmosphere of 0.1-0.15atm for 2 hours to ensure complete removal of the microbubbles.
The epoxy resin is cold-inlaid epoxy resin of Danish Tel EpoFix Kit, and the resin is completely solidified at room temperature for 12 hours without shrinkage, and is particularly suitable for vacuum impregnation and transparent in material.
(2) After curing for 2.5 hours at room temperature, when the hardness reached 20% of the hardness after complete curing, the sample was taken from the resin that was not completely cured and curing was continued for 12 hours. And directly taking out the sample before the resin is completely cured, and directly polishing the cross section of the material by using an ion beam polishing machine.
And after the solidification is finished, carrying out carbon spraying treatment on the surface of the sample to form a conductive layer, so that electron microscope observation is facilitated.
(3) Observing and selecting a proper polished section area by using an electron microscope, and alternately cutting and scanning a sample by adopting a focused ion beam-scanning electron microscope (FIB-SEM) double-beam technology to obtain a continuous two-dimensional image stream, as shown in figure 1; then, the cut picture stream is aligned by adopting an image registration technology, the image is subjected to shading correction by adopting a gray level processing technology, the two-dimensional picture is subjected to material region segmentation according to the material contrast difference, and finally, the micro-nano three-dimensional structure of the porous composite material is reconstructed based on the segmented two-dimensional digitized image, as shown in fig. 2, and the method can be adopted as the method in the prior art. Further, the processing can be performed at a later stage to obtain a three-dimensional reconstruction after the processing shown in fig. 3, and the partial schematic diagram is shown in fig. 4.
Comparative example 1
In this comparative example, unlike example 1, when filling is performed, the atmospheric pressure of the vacuum condition is greater than 0.2atm, and the obtained partial schematic diagram of the three-dimensional reconstruction is shown in fig. 5, and it can be seen that some places remain in the partial schematic diagram, and the filling is insufficient, so that the three-dimensional reconstruction of the internal structure of the material is greatly disturbed.
Comparative example 2
In this comparative example, the same type of acrylic cold set resin AK-5000 was used to fill the voids of the sample, as in example 1. Acrylic resin AK-5000 is a translucent resin with short curing time and extremely low shrinkage. The acrylic resin has good permeability to cracks and pores.
The partial schematic diagram of the three-dimensional reconstruction obtained in this comparative example is shown in fig. 6, in which the color depth varies in the place indicated by the arrow, and the structure of this part is such that the acrylic resin cannot sufficiently fill the voids and thus the resin holes remain after the resin is cured.
As can be seen from comparison of fig. 4, fig. 5 and fig. 6, the three-dimensional graph obtained by adopting the technical scheme of the invention has accurate reaction on the micro-nano structure inside the composite material, and the background image in the pore is perfectly converted into the black background with zero contrast under the observation of an electron microscope, so that the interference effect caused by the pore background can be completely solved.
The foregoing is a further detailed description of the invention in connection with the preferred embodiments, and it is not intended that the invention be limited to the specific embodiments described. It will be apparent to those skilled in the art that several simple deductions or substitutions may be made without departing from the spirit of the invention, and these should be considered to be within the scope of the invention.
Claims (4)
1. The three-dimensional reconstruction method for the micro-nano structure of the porous composite material is characterized by comprising the following steps of:
step S1, filling pores of a sample to be tested by adopting a mixture containing epoxy resin and a curing agent under a vacuum condition; the epoxy resin is EpoFix Kit cold-inlaid epoxy resin, and when the mixture of the epoxy resin and the curing agent flows through the surface of a sample to be tested to fill pores, the flow rate of the mixture of the epoxy resin and the curing agent is not more than 0.25mm/s; vacuum degree is 0.1-0.15 atm;
s2, before the epoxy resin is completely cured, taking out a sample to be tested from the incompletely cured resin, and directly polishing the section of the material by using an ion beam polishing machine; the method comprises the steps of firstly curing for 1-3 hours at room temperature, taking out a sample from the incompletely cured resin when the hardness of the epoxy resin reaches 15-25% of the hardness of the completely cured resin, and continuing curing;
and S3, observing and selecting a polished cross section area by using an electron microscope, alternately cutting and scanning a sample by using a focused ion beam-scanning electron microscope to obtain a continuous two-dimensional image stream, then carrying out alignment treatment on the two-dimensional image stream, carrying out shadow correction on an image, carrying out material area segmentation on the two-dimensional image according to the material contrast difference, and finally reconstructing a micro-nano three-dimensional structure of the porous composite material based on the segmented two-dimensional digitized image.
2. The method according to claim 1, wherein in step S1, the sample to be measured is immersed in a mixture containing epoxy resin and curing agent to fill pores, or the mixture containing epoxy resin and curing agent is used to flow over the surface of the sample to be measured to fill pores.
3. The three-dimensional reconstruction method for a micro-nano structure of a porous composite material according to claim 1, wherein step S1 further comprises allowing the filled sample to be measured to stand for 2 hours under an environment of 0.1-0.15atm, and then curing.
4. The three-dimensional reconstruction method for the micro-nano structure of the porous composite material according to claim 1, wherein after polishing in step S2 is completed, carbon spraying treatment is performed on the surface of the sample to be tested.
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| CN202010392266.0A CN111583153B (en) | 2020-05-11 | 2020-05-11 | Three-dimensional reconstruction method for micro-nano level structure of porous composite material |
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| CN108088864B (en) * | 2017-12-15 | 2020-07-14 | 浙江隆劲电池科技有限公司 | Method and system for reconstructing three-dimensional microstructure of material |
| CN108682020B (en) * | 2018-04-28 | 2019-04-12 | 中国石油大学(华东) | Rock core micron CT pore structure reconstructing method |
| CN109298005B (en) * | 2018-08-15 | 2019-06-28 | 中国科学院地质与地球物理研究所 | Focused ion beam-helium ion microscope is to shale nanoaperture three-D imaging method |
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