Shale lithofacies mineral composition measuring device
By integrating XRD and SEM sample holders into a sample base, in-situ transfer of shale lithofacies mineral composition determination was achieved, solving the problems of easy sample loss and data mismatch, and improving detection efficiency and result accuracy.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-12-05
- Publication Date
- 2026-04-03
AI Technical Summary
In existing shale lithofacies mineral composition determination techniques, the separation of sample preparation and detection processes between XRD and SEM leads to cumbersome sample handling, easy loss and contamination, making it difficult to maximize sample utilization and achieve accurate data correspondence.
A sample base integrating XRD and SEM sample cells is designed. Sample powder is transported through internal channels to achieve in-situ transfer of samples within the same sample base. The flip plate and channel design ensure stable transfer and uniform distribution of samples.
It reduces losses and contamination during base replacement and sample transfer, improves data comparability and the accuracy of test results, and reduces operational complexity and cost.
Smart Images
Figure CN121784040A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of rock and mineral analysis technology, specifically to a device for determining the mineral composition of shale lithofacies. Background Technology
[0002] Determining the mineral composition of shale lithofacies is a crucial step in shale oil and gas exploration and geological research, aiming to accurately analyze the mineral composition, content, and microstructure of shale. This process typically requires the use of multiple analytical methods, with X-ray diffraction (XRD) analysis and scanning electron microscopy (SEM) observation being two core techniques. XRD analysis provides information on the bulk mineral composition and quantitative content of the sample, forming the basis for mineral composition determination; while SEM observation reveals the microscopic morphology, distribution, and pore structure of minerals. Accurately correlating and comparing the results of these two analyses—achieving a one-to-one correspondence from "bulk composition" to "microscopic morphology"—is of paramount importance for a deeper understanding of shale genesis, reservoir properties, and fracturing resilience.
[0003] However, existing measurement techniques have significant limitations. Traditional methods require separate sample preparation and delivery for XRD and SEM analyses: first, shale powder is filled into the powder chamber of a dedicated XRD sample holder for analysis; then, some powder is removed and re-prepared onto a SEM sample holder coated with conductive adhesive before being sent for electron microscopy. This separate process is cumbersome for certain precious or rare shale samples, and the multiple sample preparation and transfer processes easily lead to sample loss, contamination, or waste, making it difficult to maximize sample utilization.
[0004] Therefore, there is an urgent need in this field for an innovative technical solution that can integrate the sample preparation and detection processes of XRD and SEM into one, so as to achieve non-destructive and accurate in-situ transfer of samples between the two detection devices. Summary of the Invention
[0005] To address the aforementioned issues, this invention provides a device for determining the mineral composition of shale lithofacies. By integrating XRD and SEM sample cells and utilizing an internal channel to transport sample powder, it achieves in-situ transfer of samples within the same sample base, thus solving the technical challenge of sample loss during cross-device testing.
[0006] To achieve the above objectives, the technical solution of the present invention is as follows: A shale lithofacies mineral composition determination device includes a sample base, which includes a first base and a second base. The first base is sleeved on the outer wall of the second base. The first base and the second base are respectively provided with a first channel and a second channel that are interconnected. A corrugated pipe is provided in the first channel. A partition is provided at the connection between the first channel and the second channel. The two ends of the corrugated pipe are respectively fixedly connected to the inner top wall of the first base and the partition. The partition has several connecting holes. A fixing rod is fixedly connected to one side of the partition located in the first channel. A powder trough for XRD detection is opened on the outer top wall of the first base. A through groove communicating with the first channel is opened at the center of the powder trough. The top of the fixing rod extends through the through groove into the powder trough, and a hemispherical sealing cap is fixedly connected to the top of the fixing rod. A spring is sleeved on the fixing rod, and the two ends of the spring are fixedly connected to the sealing cap and the partition respectively. The second base has a flip plate for SEM detection on its outer bottom wall. The flip plate has flipping components on both sides for flipping the flip plate to the front or back. The front of the flip plate has a conductive adhesive groove.
[0007] The technical principles of the above solution are as follows: The powder sample is placed in the powder tank. At this point, the spring is in its natural state, pushing the sealing cap to tightly seal the channel and prevent powder leakage. The sample base is placed in the XRD equipment. Since XRD testing often requires a base thickness of 8mm, the sleeve design of the first and second bases, combined with the flexibility of the bellows, allows the sample base to adaptively compress or expand. After XRD testing, the sample base is removed, but the powder sample remains in the powder tank. The operator applies conductive adhesive to the conductive adhesive groove on the front of the flip plate. Then, the flip plate is manually flipped using the flip assembly so that its front faces inward. As the flip plate moves inward, its edge pushes against the partition, forcing the partition to move upward along the first channel. The upward movement of the partition causes the fixing rod to rise, compressing the spring. Simultaneously, the sealing cap disengages from the channel, opening the connection between the powder tank and the first channel. Under gravity, the powder in the powder tank enters the first channel through the channel. Once the flip plate is fully flipped and fixed, the spring's restoring force pushes the partition downward to reset, causing the sealing cap to reseal the channel and prevent powder residue or leakage. The operator manually shakes the sample base, causing the sample powder remaining on the partition to enter the second channel through the connecting holes. The sample powder eventually reaches the conductive adhesive surface on the front of the flip plate and adheres evenly. The sample base is then placed in the SEM equipment. The flip plate becomes the sample stage for SEM detection, allowing direct observation of the powder sample on the conductive adhesive. Because the design of the second base and the flip plate is adapted to the SEM thickness requirements, the overall thickness of the sample base is adjusted by the relative sliding of the first and second bases.
[0008] The above approach has the following beneficial effects: 1. In traditional testing, XRD and SEM require different dedicated bases, necessitating frequent base changes and sample transfers, resulting in a cumbersome and error-prone process. This solution utilizes a sliding joint between the first and second bases, combined with the expandable and contractile properties of the corrugated tube within the first channel. This allows for adaptive adjustment of the overall thickness of the sample base to meet the clamping thickness requirements of different devices, satisfying both the standard 8mm thickness requirement for XRD and the flexible thickness requirements of SEM. Eliminating the need for multiple bases for different devices, operators can complete cross-device testing with just one device, significantly reducing the time spent on base changes and equipment setup, and lowering operational complexity and the probability of human error.
[0009] 2. In traditional methods, samples must be removed from the XRD substrate and transferred to the SEM substrate. This not only easily leads to sample loss but also completely loses the initial position information of the sample, making it impossible to accurately correspond between the volumetric data of XRD and the micro-area observation data of SEM, resulting in poor data comparability. In this scheme, the sample is placed in the powder tank during XRD detection. During transfer, a flip plate moves the partition and opens the through slot. The powder enters the second channel under gravity and adheres to the conductive adhesive on the flip plate. Throughout the process, the coordinates of the sample relative to the substrate remain unchanged, achieving an accurate correspondence between XRD volumetric data and SEM micro-area data, significantly improving data comparability. At the same time, the same shale powder sample can be used for both tests sequentially without the need for repeated sample preparation. This effectively reduces sample waste and lowers detection costs, especially for expensive shale powder.
[0010] 3. In this solution, leakage, contamination, or uneven distribution during sample transfer can directly affect the accuracy of the test results. This solution ensures sample transfer stability through multiple structural designs: First, during the XRD detection stage, the spring, in its natural state, pushes the hemispherical sealing cap to tightly seal the channel, completely preventing sample leakage from the powder tank into the channel and ensuring a stable sample volume during XRD detection. Second, during the sample transfer stage, when the flip plate flips and pushes the partition plate upward, the channel only opens during the transfer process. After the partition plate resets, the sealing cap immediately reseals the channel, preventing residual sample in the channel from contaminating subsequent tests or allowing external impurities to enter and affect sample purity. Third, by manually shaking the base in conjunction with the connecting holes on the partition plate, the sample powder remaining on the partition plate can fall evenly into the second channel and ultimately adhere evenly to the conductive adhesive surface, avoiding powder accumulation or uneven distribution. During SEM detection, a uniformly distributed sample ensures stable electronic signals, reduces detection errors caused by differences in sample distribution, and significantly improves the accuracy of SEM detection results.
[0011] Furthermore, the powder trough has a concave structure and a depth of 2-5mm. The diameter of the powder trough opening is adapted to the sample carrying specifications for XRD testing.
[0012] Beneficial effects: By precisely matching the size of the powder chamber to the specifications of the standard XRD sample holder, the standardization and comparability of the test data are ensured.
[0013] Furthermore, the flipping assembly includes a rotating shaft, both ends of which are rotatably connected to the second base, and the rotating shaft is fixedly connected to the horizontal direction of the flipping plate.
[0014] Beneficial effects: The use of a rotating shaft connection enables stable and precise flipping of the flip plate. This structure ensures that the flipping action is performed around a fixed axis, avoiding shaking or offset during the flipping process. This guarantees that the conductive adhesive fixed on the flip plate and the powder sample it adheres to can accurately and reliably reach the preset SEM detection position, improving the repeatability and success rate of the operation.
[0015] Furthermore, the conductive adhesive adhesive groove is symmetrically provided with limiting bosses for defining the position of the conductive adhesive adhesive.
[0016] Beneficial effects: The limiting boss provides a clear physical reference for applying conductive adhesive, ensuring that the adhesive can be quickly and accurately applied to the predetermined position each time. This eliminates positional errors that may be caused by manual application, ensuring that the coordinates of the SEM observation area relative to the sample base remain constant. This is a key detail in maintaining the spatial correspondence between XRD and SEM data.
[0017] Furthermore, the second base has a slot on its bottom side wall, and the flip plate has an elastic buckle corresponding to the slot.
[0018] Beneficial effects: The combination of the elastic buckle and the slot ensures that the flip plate is securely locked in its working position after it has been flipped. This locking mechanism prevents the flip plate from accidentally loosening or rotating during subsequent handling or placement on the SEM sample stage, ensuring the stability of the detection process and the safety of the sample.
[0019] Furthermore, the second base is provided with several sliding grooves, and the first base is provided with sliders that correspond one-to-one with the sliding grooves and slide in cooperation with them.
[0020] Beneficial effects: The sliding fit between the slider and the groove provides precise guidance for the relative movement of the first and second bases. This not only prevents rotation or misalignment during sliding, ensuring the powder channel is always aligned, but also makes the thickness adjustment process of the bases smoother and more stable, enhancing the structural rigidity and operational feel of the entire device.
[0021] Furthermore, both the first and second bases are equipped with connection interfaces for XRD and SEM inspection equipment on their outer sides, and each connection interface is equipped with a positioning pin.
[0022] Beneficial effects: The standardized connection interface and positioning pin design enable the sample base to be used as a universal carrier and quickly and accurately installed on the sample stage of different testing equipment.
[0023] Furthermore, the edge of the powder trough is integrally formed with a horizontal calibration scale line, the line width of which is 0.2-0.4mm.
[0024] Beneficial effects: The horizontal calibration scale lines provide an intuitive visual reference for leveling powder during sample preparation. The 0.2-0.4mm line width is clearly visible without being too wide and affecting the leveling accuracy. By ensuring that the powder surface is flush with the scale lines, the uniformity of the sample surface during XRD detection can be guaranteed, thereby obtaining higher quality and more reliable diffraction patterns.
[0025] Furthermore, a sealing cap is detachably connected to the opening of the powder trough.
[0026] Beneficial effects: The sealing cap can effectively prevent the powder from being lost or deteriorated due to accidental spillage, moisture or contamination during transfer and operation after XRD detection and before SEM sample preparation. It has important practical value for preserving valuable samples and ensuring the effectiveness of subsequent SEM analysis.
[0027] Furthermore, anti-slip silicone pads are fixedly connected to the four corners of the outer bottom wall of the second base, and the thickness of the anti-slip silicone pads is 1-2mm.
[0028] Beneficial effects: The anti-slip silicone pad increases the friction between the base and the sample stage or workbench surface, preventing the sample base from accidentally sliding during placement or operation, thus improving operational safety. At the same time, the soft silicone pad can also prevent scratches on the surface of the precision equipment sample stage. Attached Figure Description
[0029] Figure 1 This is a front axonometric schematic diagram of an embodiment of the shale lithofacies mineral composition determination device of the present invention; Figure 2 This is a front cross-sectional schematic diagram of an embodiment of the shale lithofacies mineral composition determination device of the present invention; Figure 3 This is a reverse isometric schematic diagram of an embodiment of the shale lithofacies mineral composition determination device of the present invention.
[0030] The reference numerals in the accompanying drawings of the instruction manual include: 1. First base; 2. Powder tank; 3. Sealing cap; 4. Second base; 5. Slider; 6. Slide groove; 7. Flip plate; 8. Rotating shaft; 9. Second channel; 10. Through hole; 11. Partition plate; 12. First channel; 13. Bellows; 14. Spring; 15. Fixing rod; 16. Conductive adhesive groove; 17. Limiting boss. Detailed Implementation
[0031] The technical solution of the present invention will now be clearly and completely described with reference to the accompanying drawings. Obviously, the described embodiments are only some, not all, of the embodiments of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0032] In the description of this invention, it should be noted that the terms "center," "upper," "lower," "left," "right," "vertical," "horizontal," "inner," and "outer," etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are used only for the convenience of describing the invention and for simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on the invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and should not be construed as indicating or implying relative importance.
[0033] In the description of this invention, it should be noted that, unless otherwise explicitly specified and limited, the terms "installation," "connection," and "linking" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; and they can refer to the internal connection of two components. Those skilled in the art can understand the specific meaning of the above terms in this invention based on the specific circumstances.
[0034] The following detailed description illustrates the specific implementation method: Example:
[0035] In the field of shale lithofacies mineral composition determination, traditional methods typically require powder samples to be sent separately to X-ray diffraction (XRD) and scanning electron microscopy (SEM) equipment for independent analysis. Because XRD and SEM use different sample substrates and preparation requirements, positional information is easily lost during sample transfer, leading to inaccurate correlations between XRD volumetric data and SEM microscopic observations. Furthermore, shale powder samples are expensive, and traditional preparation processes can result in sample loss or contamination, making sample reuse and in-situ comparisons difficult. These problems severely limit analytical efficiency and data reliability, especially when multi-device collaborative analysis is required, resulting in cumbersome operations and significant errors.
[0036] Therefore, the inventor proposed the following: Figure 1The device shown is for determining the mineral composition of shale lithofacies, achieving in-situ integration of XRD and SEM detection, ensuring the uniqueness and comparability of sample locations. Taking a shale exploration project as an example, researchers need to analyze the mineral composition (via XRD) and microstructure (via SEM) of the same powder sample. Specifically, it includes a sample base, comprising a first base 1 and a second base 4. The first base 1 is fitted onto the outer wall of the second base 4. The second base 4 has several grooves 6, and the first base 1 has sliders 5 that correspond one-to-one with and slide in cooperation with the grooves 6, as shown in the attached diagram. Figure 2 As shown, the first base 1 and the second base 4 are respectively provided with a first channel 12 and a second channel 9 that are interconnected. The first channel 12 is provided with a corrugated pipe 13. A partition 11 is provided at the connection between the first channel 12 and the second channel 9. The two ends of the corrugated pipe 13 are fixedly connected to the inner top wall of the first base 1 and the top wall of the partition 11, respectively. The partition 11 has a plurality of connecting holes 10. A fixing rod 15 is fixedly connected to one side of the partition 11 located in the first channel 12. The outer top wall of the first base 1 has a powder trough 2 for XRD detection. The powder trough 2 has a concave structure and a sealing cover can be detachably connected to the trough opening. The depth of the powder trough 2 is 2-5mm, and the diameter of the trough opening is adapted to the sample carrying specifications for XRD detection. The edge of the trough opening of the powder trough 2 has an integrally formed horizontal calibration scale line with a line width of 0.2-0.4mm.
[0037] A through groove communicating with the first channel 12 is opened at the center of the powder tank 2. The top end of the fixing rod 15 extends through the through groove into the powder tank 2, and a hemispherical sealing cap 3 is fixedly connected to the top end of the fixing rod 15. A spring 14 is sleeved on the fixing rod 15, and the two ends of the spring 14 are fixedly connected to the sealing cap 3 and the partition plate 11 respectively. The outer bottom wall of the second base 4 is provided with a flip plate 7 for SEM inspection. Flipping components for flipping the flip plate 7 to the front or back are provided on both sides of the flip plate 7. Each flipping component includes a rotating shaft 8, both ends of which are rotatably connected to the second base 4, and the rotating shaft 8 is fixedly connected to the horizontal direction of the flip plate 7, as shown in the attached figure. Figure 3 As shown, the front of the flip plate 7 has a conductive adhesive groove 16, and the conductive adhesive groove 16 is symmetrically provided with limiting protrusions 17 for limiting the position of the conductive adhesive. The bottom side wall of the second base 4 is provided with a slot, and the flip plate 7 is provided with an elastic buckle corresponding to the slot. Anti-slip silicone pads are fixedly connected to the four corners of the outer bottom wall of the second base 4, and the thickness of the anti-slip silicone pads is 1-2mm.
[0038] Both the outer sides of the first base 1 and the second base 4 are provided with connection interfaces for XRD and SEM inspection equipment, and each connection interface is provided with a positioning pin.
[0039] When using this device, first place the sample base on the XRD testing equipment. The powder sample is placed into the powder trough 2 on the outer top wall of the first base 1. The powder trough 2 has a depth of 3mm, and its opening diameter is adapted to the standard XRD sample carrying specifications to ensure uniform sample distribution. The horizontal calibration scale lines on the edge of the powder trough 2's opening are used to assist in placement, ensuring the sample is level and avoiding X-ray detection deviation. The sealing cap is removable and is used to seal the powder trough 2 before testing to prevent contamination.
[0040] After XRD analysis, researchers need to transfer the same sample to SEM analysis. At this point, researchers manually operate the flip plate 7. As the rotating shaft 8 rotates, the flip plate 7 flips from the outer bottom wall of the second base 4 into the second channel 9. The front of the flip plate 7 has a conductive adhesive groove 16, with symmetrically arranged limiting protrusions 17 inside the groove to fix the position of the conductive adhesive and ensure even adhesion. When the flip plate 7 begins to flip, its mechanical structure moves upward along the first channel 12 via the pushing partition 11. The partition 11 drives the fixing rod 15 to compress the spring 14, causing the hemispherical sealing cap 3 at the top of the fixing rod 15 to disengage from the through groove at the bottom of the powder tank 2. This linkage opens the communication path between the powder tank 2 and the first channel 12. Under gravity, the powder enters the first channel 12 through the through groove. After the powder enters the first channel 12, the flip plate 7 continues to flip until it is completely closed, and the elastic buckle embeds into the slot on the side wall of the second base 4, fixing the position of the flip plate 7. Simultaneously, the partition 11 resets under the action of the spring 14, and the sealing cap 3 re-blocks the through-slot to prevent powder leakage. The operator manually shakes the sample base, allowing the sample powder to enter the second channel 9 through the through-hole 10 from the partition 11. This achieves the most uniform distribution of the powder sample as possible, given that the conductive adhesive has already adhered to the powder. At this point, the sample base can be directly moved to the SEM detection equipment. The flipping plate 7 is then operated to ensure the powder-coated side faces outwards, and the anti-slip silicone pad ensures stable placement of the base. The connecting interface and positioning pins ensure precise docking of the base with the SEM equipment, guaranteeing that the observation area is consistent with that used in XRD detection. The entire process requires no manual transfer of the powder sample; the flipping action and channel design achieve uniform powder delivery and adhesion, reducing sample loss.
[0041] Furthermore, the first base 1 and the second base 4, through the sliding engagement of the slider 5 and the groove 6, and the extensibility of the bellows 13, adjust their overall height to accommodate the different thickness requirements of XRD and SEM equipment. For example, XRD equipment typically requires a thicker base (e.g., 8 mm), while SEM equipment requires a thinner one. The bellows 13 is compressed or extended within the first channel 12 to ensure that the sample position remains constant relative to the base coordinates. This design avoids positional shifts caused by base replacement in traditional methods, improving data comparability and reusability.
[0042] Obviously, the above embodiments are merely illustrative examples for clear explanation and are not intended to limit the implementation. Those skilled in the art will recognize that other variations or modifications can be made based on the above description. It is neither necessary nor possible to exhaustively list all possible implementations here. However, obvious variations or modifications derived therefrom are still within the scope of protection of this invention.
Claims
1. A device for determining the mineral composition of shale lithofacies, characterized in that, The sample base includes a first base (1) and a second base (4). The first base (1) is fitted onto the outer wall of the second base (4). The first base (1) and the second base (4) are respectively provided with a first channel (12) and a second channel (9) that are interconnected. A corrugated pipe (13) is provided in the first channel (12). A partition (11) is provided at the connection between the first channel (12) and the second channel (9). The two ends of the corrugated pipe (13) are fixedly connected to the inner top wall of the first base (1) and the partition (11) respectively. Several connecting holes (10) are opened on the partition (11). A fixing rod (15) is fixedly connected to one side of the partition (11) located in the first channel (12). The first base (1) has a powder trough (2) for XRD detection on its outer top wall. The powder trough (2) has a through groove at its center that communicates with the first channel (12). The top of the fixing rod (15) extends through the through groove into the powder trough (2). A hemispherical sealing cap (3) is fixedly connected to the top of the fixing rod (15). A spring (14) is sleeved on the fixing rod (15). The two ends of the spring (14) are fixedly connected to the sealing cap (3) and the partition (11) respectively. The second base (4) has a flip plate (7) for SEM detection on its outer bottom wall. The flip plate (7) has flip components on both sides for flipping the flip plate (7) to the front or back. The flip plate (7) has a conductive adhesive groove (16) on its front side.
2. The shale lithofacies mineral composition determination device according to claim 1, characterized in that, The powder trough (2) has a concave structure and a depth of 2-5 mm. The diameter of the trough opening of the powder trough (2) is adapted to the sample carrying specifications for XRD detection.
3. The apparatus for determining the mineral composition of shale lithofacies according to claim 2, characterized in that, The flipping assembly includes a rotating shaft (8) with both ends of the rotating shaft (8) rotatably connected to the second base (4), and the rotating shaft (8) is fixedly connected to the flipping plate (7) in the horizontal direction.
4. The shale lithofacies mineral composition determination device according to claim 3, characterized in that, The conductive adhesive adhesive groove (16) is symmetrically provided with limiting bosses (17) for limiting the position of the conductive adhesive adhesive.
5. The apparatus for determining the mineral composition of shale lithofacies according to claim 4, characterized in that, The second base (4) has a slot on its bottom side wall, and the flip plate (7) has an elastic buckle corresponding to the slot.
6. The apparatus for determining the mineral composition of shale lithofacies according to claim 5, characterized in that, The second base (4) is provided with several sliding grooves (6), and the first base (1) is provided with sliders (5) that correspond one-to-one with the sliding grooves (6) and slide together.
7. The apparatus for determining the mineral composition of shale lithofacies according to claim 6, characterized in that, Both the outer sides of the first base (1) and the second base (4) are provided with connection interfaces for XRD detection equipment and SEM detection equipment, and positioning pins are provided at the connection interfaces.
8. The apparatus for determining the mineral composition of shale lithofacies according to claim 7, characterized in that, The edge of the powder trough (2) is integrally formed with a horizontal calibration scale line, and the line width of the horizontal calibration scale line is 0.2-0.4mm.
9. The apparatus for determining the mineral composition of shale lithofacies according to claim 8, characterized in that, A sealing cap is detachably connected to the opening of the powder trough (2).
10. The apparatus for determining the mineral composition of shale lithofacies according to claim 9, characterized in that, Anti-slip silicone pads are fixedly connected to the four corners of the outer bottom wall of the second base (4), and the thickness of the anti-slip silicone pads is 1-2mm.