CN108051462B - micro-CT multi-sample preparation device and using method - Google Patents
micro-CT multi-sample preparation device and using method Download PDFInfo
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- CN108051462B CN108051462B CN201711281160.8A CN201711281160A CN108051462B CN 108051462 B CN108051462 B CN 108051462B CN 201711281160 A CN201711281160 A CN 201711281160A CN 108051462 B CN108051462 B CN 108051462B
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- 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
- G01N23/02—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 transmitting the radiation through the material
- G01N23/04—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 transmitting the radiation through the material and forming images of the material
- G01N23/046—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 transmitting the radiation through the material and forming images of the material using tomography, e.g. computed tomography [CT]
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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Abstract
The invention provides a micro CT multi-sample preparation device and a method, wherein the micro CT multi-sample preparation device comprises: support, sample bracing piece, coaxial protector, paraffin, depression bar. The position of a sample combination body formed by a plurality of samples is corrected by adopting the coaxial protector sleeve on the sample supporting rod, so that the samples cannot exceed the extension line range of the sample supporting rod, and the rotating diameter of all samples during testing is not more than the diameter of the sample supporting rod. The adhesive paraffin is used as an adhesive material, so that a plurality of samples can be conveniently and quickly adhered together and then are firmly adhered to the sample supporting rod, the samples can be conveniently filtered in subsequent image processing, and the samples are easily taken down and separated after the test is finished and cannot be damaged. The equipment is simple, the operation is convenient, and the time and the labor are saved.
Description
Technical Field
The invention relates to a sample preparation method, in particular to a micro-CT multi-sample preparation device and a using method thereof.
Background
Micro-CT (Micro-Computed Tomography), also known as X-ray microtomography. Refers to CT with spatial resolution up to about lum. The main components of the micro CT comprise an X-ray source, a rotary sample stage and a high-resolution detector. The X-ray source and the detector are fixed, the sample rotates between the X-ray source and the detector, and the X-ray source generates a continuous conical X-ray beam which penetrates through the sample to be detected and is imaged on the X-ray detector. By rotating the sample at an angular rate, x-ray projections of the sample at different angles are obtained. And reconstructing the projection image of each angle through corresponding computer software, and restoring the projection image into a 3D image which can be analyzed in a computer. In order to achieve higher resolution, the step length during rotation is smaller, the exposure time is longer, and in order to improve definition and accuracy, a plurality of images are acquired at each angle for image fusion and correction, so that the parameter debugging and image acquisition time of the micro CT is very long. In the routine microscopic CT scanning analysis, if only one sample is made at a time, the scanning efficiency is very low, and the loss of the instrument is large when the ray and the sample bin gate are frequently opened and closed. Therefore, in order to save time and improve testing efficiency, several samples with similar X-ray absorption coefficients are often placed on a sample stage to be tested simultaneously. Due to the limited area of the CCD or other detector used for image acquisition, in order to observe as large (a large) sample volume (quantity) as possible within the limited (CCD) field of view, it is necessary to ensure that the sample is brought towards the axis of the instrument rotation stage. Because the instrument revolving stage diameter is great, the sample need be through the bracing piece connection revolving stage with the revolving stage is coaxial. Therefore, the sample must be centered as far as possible on the sample support rod, and the rotation diameter is not larger than the support rod diameter.
Because the quantity of the existing micro CT is less, the sample preparation devices are not many, the sample easily exceeds the diameter range of the supporting rod by the conventional sample preparation means, the success rate is not high, and the requirement of the micro CT on quick sample preparation of multiple samples cannot be met.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a micro-CT multi-sample preparation device and a method, so that the rotating diameter of a sample does not exceed the diameter of a sample supporting rod.
Detailed Description
The invention provides a micro-CT multi-sample preparation device, which comprises: the device comprises a support 6, a sample supporting rod 1, a coaxial protector 2, paraffin 3 and a pressure rod 5.
The support 6 is a stable four-leg support with a horizontal table top and a height adjuster 7, a hole capable of penetrating the sample supporting rod 1 is formed in the middle of the table top, and the size of the table top ensures that the coaxial protector can be completely placed.
The coaxial protector 2 is a thick-wall round tube capable of being opened and closed, and consists of two semicircular tubes, a positioning device is arranged at the closing position, the inner wall of the round tube is smooth, the inner diameter of the round tube is the same as the diameter of one end of the supporting rod for containing a sample, the height of the round tube is 30-100mm, the wall thickness of the round tube is 5-10mm, and the round tube is made of polytetrafluoroethylene.
The paraffin 3 has certain viscosity and plasticity, and can fix (stick) the sample and the sample supporting rod 1 together, and the sample cannot rebound after the external force is cancelled.
The pressure bar 5 is a cylinder, the diameter of the pressure bar is slightly smaller than the inner diameter of the coaxial protector 2, the pressure bar can freely move in the coaxial protector 2, and the pressure bar is made of polytetrafluoroethylene.
By utilizing the device, the invention provides a method for preparing a plurality of samples by using micro CT, which comprises the following steps:
1. each sample is processed into a cuboid shape with appropriate size and height according to the requirement of certain resolution micro CT test (for the sample which is difficult to process, other shapes are also possible). The method comprises the steps of adhering proper paraffin to two ends of a plurality of samples to be tested, then tightly gathering the samples together, and adhering the samples into an assembly through the paraffin at the two ends, wherein the diameter of the assembled sample 4 which is gathered together is minimized as much as possible.
2. In order to ensure a high resolution and a large effective viewing range, the support rods are selected to be as thin as possible on the premise of accommodating the sample assembly 4 to be measured. Vertically placing the sample supporting rod 1 into a hole in the middle of the table top of the bracket 6, filling a proper amount of paraffin 3 into a groove 8 at the top end of the sample supporting rod 1, and filling 1/2 of the groove, and compacting. Then vertically placing the sample combination 4 on the paraffin in the groove 8, continuously adding a proper amount of paraffin, filling the groove, and burying the bottom of the sample combination 4 into the groove 8 for fixing.
3. The coaxial protector 2 is separately placed on the table surface of the bracket at two sides of the sample supporting rod, and the height of the bracket 6 is adjusted by the bracket height adjuster 7, so that the top end of the sample assembly 4 is lower than the top end of the coaxial protector 2.
4. The coaxial protector 2 is closed and tightly sleeved on the sample supporting rod, and the sample combination body is corrected to be within the diameter range of the sample supporting rod. Then, the sample assembly 4 is slightly pressed downwards by the pressing rod 5, so that the position of the sample assembly 4 is more stable.
5. The coaxial protector 2 is carefully separated outwards to expose the sample supporting rod 2 and the sample assembly 4, paraffin 3 at the bottom of the sample assembly 4 is accumulated on the sample 4 by using a proper tool such as a toothpick, the sample assembly 4 is firmly fixed on the sample supporting rod 1, and the paraffin 1 cannot exceed the sample supporting rod.
6. And (3) closing the coaxial protector 2 on the sample supporting rod 1 again, if the sample assembly 4 exceeds the diameter range of the sample supporting rod due to the previous operation, adjusting the sample assembly back, standing for 3-5 minutes, then removing the coaxial protector 2, and compacting the paraffin 3 at the bottom of the sample assembly 4 by using a proper tool such as a toothpick.
7. And (6) repeating the step until the combination of the bottom of the sample assembly and the paraffin is unchanged after the coaxial protector 2 is taken down, and finishing the preparation of the sample.
Advantageous effects
The coaxial protector sleeve is adopted to correct the position of a sample combination body formed by a plurality of samples by the sample supporting rod, so that the samples are ensured not to exceed the extension line range of the sample supporting rod, and the rotating diameter of all samples during testing is ensured not to exceed the diameter of the sample supporting rod. The equipment is simple, the operation is convenient, and the time and the labor are saved. The adhesive paraffin wax which is a low-density substance composed of C, H elements is used as an adhesive material, so that a plurality of samples can be conveniently and quickly adhered together and then are firmly adhered to the sample supporting rod, the samples can be conveniently filtered in subsequent image processing, and the samples are easily taken down and separated after the test is finished and cannot be damaged.
Drawings
FIG. 1 is a schematic diagram of a longitudinal section of a micro-CT multi-sample preparation device according to the present invention;
FIG. 2 is a schematic diagram showing the structure of a longitudinal section of a groove formed at the tip of a sample support rod according to the present invention.
The device comprises a sample supporting rod 1, a coaxial protector 2, paraffin 3, a sample assembly 4, a pressure rod 5, a support 6, a support height adjuster 7 and a sample supporting rod groove 8.
Detailed Description
The invention is further illustrated with reference to the following examples and the accompanying drawings of the description, without limiting the scope of the invention thereto.
The embodiment of the invention provides a micro-CT multi-sample preparation device, which comprises: the device comprises a support 6, a sample supporting rod 1, a coaxial protector 2, paraffin 3 and a pressure rod 5.
The support 6 is a stable four-leg support with a horizontal table top and a height adjuster 7, a hole capable of penetrating the sample supporting rod 1 is formed in the middle of the table top, and the size of the table top ensures that the coaxial protector can be completely placed.
The coaxial protector 2 is a thick-wall round pipe capable of being opened and closed, and is composed of two semicircular pipes, a positioning device is arranged at the closing position, the inner wall of the round pipe is smooth, the inner diameter is 8mm, the height is 50mm, the wall thickness is 10mm, and the material is polytetrafluoroethylene.
The paraffin 3 has certain viscosity and plasticity, can stick the sample together, is fixed (stuck) with the sample support rod 1, and can not cause the sample to rebound after the external force is cancelled.
The pressure bar 5 is a cylinder with the diameter of 7mm, can freely move in the coaxial protector 2 and is made of polytetrafluoroethylene.
By utilizing the device, the invention provides a method for preparing a plurality of samples by using micro CT, which comprises the following steps:
1. according to the requirements of micro CT test of cow leather in different processes, 4 leather samples are processed into cuboid shapes with the size of 3mm x 8 mm. After the two ends of the 4 samples are adhered with proper amount of paraffin, the samples are tightly gathered together, and the paraffin at the two ends is adhered into a combination body, so that the diameter of the combined body 4 of the samples gathered together is minimized.
2. To ensure higher resolution and a larger effective viewing range, the 8mm diameter sample support rod was chosen. Vertically placing the sample supporting rod 1 into a hole in the middle of the table top of the bracket 6, filling a proper amount of paraffin 3 into a groove 8 at the top end of the sample supporting rod 1, and filling 1/2 of the groove, and compacting. Then vertically placing the sample combination 4 on the paraffin in the groove 8, continuously adding a proper amount of paraffin, filling the groove, and burying the bottom of the sample combination 4 into the groove 8 for fixing.
3. The coaxial protector 2 is separately placed on the table surface of the bracket at two sides of the sample supporting rod, and the height of the bracket 6 is adjusted by the bracket height adjuster 7, so that the top end of the sample assembly 4 is lower than the top end of the coaxial protector 2.
4. The coaxial protector 2 is closed and tightly sleeved on the sample supporting rod, and the sample combination body is corrected to be within the diameter range of the sample supporting rod. Then, the sample assembly 4 is slightly pressed downwards by the pressing rod 5, so that the position of the sample assembly 4 is more stable.
5. The coaxial protector 2 is carefully separated outwards to expose the sample supporting rod 2 and the sample assembly 4, paraffin 3 at the bottom of the sample assembly 4 is accumulated on the sample 4 by using a proper tool such as a toothpick, the sample assembly 4 is firmly fixed on the sample supporting rod 1, and the paraffin 3 cannot exceed the sample supporting rod.
6. And (3) closing the coaxial protector 2 on the sample supporting rod 1 again, if the sample assembly 4 exceeds the diameter range of the sample supporting rod due to the previous operation, adjusting the sample assembly back, standing for 3-5 minutes, then removing the coaxial protector 2, and compacting the paraffin 3 at the bottom of the sample assembly 4 by using a proper tool such as a toothpick.
7. And (6) repeating the step until the combination of the bottom of the sample assembly and the paraffin is unchanged after the coaxial protector 2 is taken down, and finishing the preparation of the sample.
The above examples are intended to illustrate the present invention, but not to limit the present invention, and those skilled in the art can make various changes and modifications without departing from the spirit and scope of the present invention, and therefore all equivalent technical solutions should fall within the scope of the present invention, which should be limited by the claims.
Claims (2)
1. A micro-CT multi-sample preparation device, comprising: the device comprises a bracket (6), a sample supporting rod (1), a coaxial protector (2), paraffin (3) and a pressure lever (5);
the bracket is a stable four-leg bracket with a horizontal table top and a height adjuster, a hole capable of penetrating through the sample supporting rod is formed in the middle of the table top, and the size of the table top is ensured to be completely provided with the coaxial protector; the sample supporting rod is cylindrical, one end of the sample supporting rod is connected with the instrument rotating platform, one end of the sample supporting rod is used for containing a sample, a groove (8) is arranged at one end of the sample containing rod, the length and the diameter of the groove are 100-200mm according to the requirement of the instrument, the diameter of the groove is 1-10mm, further, the bottom of the groove is conical, the depth of the conical part is 1-5mm, the upper end of the groove is cylindrical, and the depth of the cylindrical part is 1-5 mm; the coaxial protector is a thick-wall round tube capable of being opened and closed, and consists of two semicircular tubes, a positioning device is arranged at the joint, the inner wall of the round tube is smooth, the inner diameter of the round tube is the same as the diameter of one end of the sample supporting rod for containing a sample, the height of the round tube is 30-100mm, the wall thickness of the round tube is 5-10mm, and the round tube is made of polytetrafluoroethylene; the paraffin has certain viscosity and plasticity, and can fix the sample and the sample supporting rod together, and the sample cannot rebound after the external force is cancelled; the depression bar is a cylinder, and its diameter slightly is lighter than coaxial protector internal diameter, can freely remove in coaxial protector, and the material is polytetrafluoroethylene.
2. A micro-CT multiple-sample preparation method, characterized in that the micro-CT multiple-sample preparation apparatus of claim 1 is used for sample preparation, comprising the following steps:
step 1, processing each sample into a cuboid shape with appropriate size and height according to the requirement of a micro CT test with certain resolution; the method comprises the following steps of adhering proper paraffin to two ends of a plurality of samples to be tested, then tightly gathering the samples together, and adhering the samples into a combined body through the paraffin at the two ends, so that the diameter of the combined body (4) of the gathered samples is minimized;
step 2, in order to ensure higher resolution and larger effective observation range, selecting the support rods which can be as thin as possible on the premise of accommodating the tested sample assembly (4); vertically placing a sample supporting rod (1) into a hole in the middle of the table top of a bracket (6), filling a proper amount of paraffin (3) into a groove (8) at the top end of the sample supporting rod (1), filling 1/2 of the groove, and compacting; then vertically placing the sample assembly (4) on paraffin in the groove (8), continuously adding a proper amount of paraffin, filling the groove, and burying the bottom of the sample assembly (4) into the groove (8) for fixing;
step 3, opening the coaxial protector (2) on the support table surfaces at two sides of the sample supporting rod, and adjusting the height of the support (6) through a support height adjuster (7) to enable the top end of the sample assembly (4) to be lower than the top end of the coaxial protector (2);
step 4, closing the coaxial protector (2), tightly sleeving the coaxial protector on the sample supporting rod, and correcting the sample assembly to ensure that the diameter of the sample assembly does not exceed the diameter range of the sample supporting rod; then, the sample combination body (4) is slightly pressed downwards by a pressure lever (5), so that the position of the sample combination body (4) is more stable;
step 5, the coaxial protector (2) is carefully separated outwards to expose the sample supporting rod (2) and the sample assembly (4), paraffin (3) at the bottom of the sample assembly (4) is accumulated on the sample (4) by using a proper tool such as a toothpick, and the sample assembly (4) is firmly fixed on the sample supporting rod (1), and the paraffin (3) cannot exceed the sample supporting rod;
step 6, the coaxial protector (2) is closed onto the sample supporting rod (1) again, if the sample assembly (4) exceeds the diameter range of the sample supporting rod due to the operation of the previous step, the sample assembly is adjusted back, the coaxial protector (2) is taken down after standing for 3-5 minutes, and paraffin (3) at the bottom of the sample assembly (4) is compacted by using a proper tool such as a toothpick;
and 7, repeating the step 6 until the combination of the bottom of the sample assembly and the paraffin is unchanged after the coaxial protector (2) is taken down, and finishing the preparation of the sample.
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| CN108051462B true CN108051462B (en) | 2020-04-21 |
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| CN109253906B (en) * | 2018-11-05 | 2023-11-17 | 东北石油大学 | Device and method for bonding and preparing micro core samples |
| CN111929094B (en) * | 2019-05-13 | 2023-11-28 | 中国石油化工股份有限公司 | Sampling device and sampling method for nano CT test sample |
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| CN102023111B (en) * | 2010-11-02 | 2012-05-16 | 大连理工大学 | Method for preparing transmission electron microscope sample of soft brittle phototransistor |
| CN103076211B (en) * | 2012-12-20 | 2015-07-29 | 华南理工大学 | Making and many wheels of right cylinder bitumen mixture specimen load wheel tracking test method |
| CN104237237B (en) * | 2014-09-29 | 2016-08-24 | 中国科学院上海应用物理研究所 | A kind of synchrotron radiation X-ray Micro CT imaging sample stage |
| CN104614935A (en) * | 2015-02-06 | 2015-05-13 | 浙江大学 | Universal high-precision micro-structure preparation system and application method of universal high-precision micro-structure |
| CN205374345U (en) * | 2015-12-25 | 2016-07-06 | 北京市创伤骨科研究所 | Computer tomoscan sample objective table |
| CN105973713B (en) * | 2016-06-28 | 2018-11-23 | 浙江理工大学 | A kind of deformation of solid refuse and intensity related assays instrument |
| CN105973674B (en) * | 2016-07-01 | 2017-03-29 | 中国科学院地质与地球物理研究所 | A kind of preparation method of the thin area's sample for use in transmitted electron microscope of large area |
| CN206435750U (en) * | 2017-02-07 | 2017-08-25 | 安吉县宏铭磁性器材有限公司 | A kind of moulding press of magnetic separator magnetic material |
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