阅读说明：本技术 一种适用于氩离子抛光的多样品制备装置及方法 (Multi-sample preparation device and method suitable for argon ion polishing ) 是由 周圆圆 俞凌杰 芮晓庆 刘友祥 张庆珍 范明 于 2019-02-21 设计创作，主要内容包括：本发明公开了一种适用于氩离子抛光的多样品制备装置及方法。该制备装置包括：底座托盘,其上设有第一通孔；顶盖,可拆卸地连接于底座托盘,顶盖上设有定位机构；样品座,设于底座托盘上,样品座上设有多个第二通孔,第二通孔用于放置岩样,当顶盖连接于底座托盘时,定位机构将岩样固定于第二通孔内；反应容器,能够容纳底座托盘。本发明通过设置有多个通孔的样品座能够单次制备多个用于氩离子抛光的岩石样品,并解决了岩石样品的固定问题,有效提高了氩离子抛光的效率、节约成本。(The invention discloses a multi-sample preparation device and method suitable for argon ion polishing. The preparation device comprises: the base tray is provided with a first through hole; the top cover is detachably connected with the base tray and is provided with a positioning mechanism; the sample seat is arranged on the base tray, a plurality of second through holes are formed in the sample seat and used for placing the rock sample, and when the top cover is connected to the base tray, the rock sample is fixed in the second through holes through the positioning mechanism; a reaction vessel capable of accommodating the base tray. According to the invention, a plurality of rock samples for argon ion polishing can be prepared at a time through the sample seat provided with a plurality of through holes, the problem of fixing the rock samples is solved, the argon ion polishing efficiency is effectively improved, and the cost is saved.)

1. A multi-sample preparation device suitable for argon ion polishing, comprising:

the base tray is provided with a first through hole;

the top cover is detachably connected to the base tray, and a positioning mechanism is arranged on the top cover;

the sample seat is arranged on the base tray, a plurality of second through holes are formed in the sample seat, the second through holes are used for placing rock samples, and when the top cover is connected to the base tray, the rock samples are fixed in the second through holes through the positioning mechanism;

a reaction vessel capable of receiving the base tray.

2. The multi-sample preparation device suitable for argon ion polishing as claimed in claim 1, wherein said first through hole is plural, and plural of said first through holes are provided at a bottom of said base tray.

3. The apparatus of claim 1, wherein the top cover has a plurality of threaded holes therethrough, each threaded hole corresponding to one of the second through-holes when the top cover is attached to the base tray, and wherein the positioning mechanism comprises a plurality of threaded pins, each threaded pin being threadedly attached within one of the threaded holes to secure the rock sample within the second through-hole.

4. The multi-sample preparation device suitable for argon ion polishing as claimed in claim 1, wherein the base tray is connected with the top cap by a screw thread, and a sealing ring is provided at the connection part of the base tray and the top cap.

5. The multi-sample preparation device suitable for argon ion polishing as claimed in claim 1, wherein the number of said first through holes is larger than the number of said second through holes; and/or

The first through hole and the second through hole are both cylindrical holes, and the diameter of the first through hole is smaller than that of the second through hole.

6. The device of claim 1, wherein the bottom surface of the base tray is coated with teflon, and/or the reaction vessel is made of teflon.

7. The multi-sample preparation device suitable for argon ion polishing as claimed in claim 1, further comprising a heater disposed below said reaction vessel.

8. The multi-sample preparation device suitable for argon ion polishing as claimed in claim 1, wherein the material of said sample holder is metal.

9. A method for preparing multiple samples suitable for argon ion polishing using the preparation apparatus of any one of claims 1 to 8, the method comprising:

step 1: placing the sample seat on the base tray, selecting a plurality of rock samples, and placing each rock sample in one second through hole to form a gap between the periphery of the rock sample and the inner wall of the second through hole;

step 2: connecting the top cover to the base tray, and fixing the rock sample in the second through hole through the positioning mechanism;

and step 3: placing the base tray in the reaction vessel, pouring molten metal into the reaction vessel and immersing the first through holes in the molten metal;

and 4, step 4: heating molten metal in the reaction vessel;

and 5: stopping heating, and taking out the sample holder after the molten metal is solidified.

10. The production method according to claim 9, wherein in the step 4, the heating temperature is higher than the melting point of the metal.

11. The production method according to claim 9, wherein in the step 3, the metal is a low melting point alloy.

12. The method of claim 9, wherein the height of the rock sample is greater than or equal to the depth of the second through hole.

Technical Field

The invention relates to the field of oil-gas exploration, in particular to a multi-sample preparation device and method suitable for argon ion polishing.

Background

The shale has abundant micron-nanometer pores inside, and a clean and flat surface can be obtained by means of an argon ion polishing technology, so that high-resolution clear imaging is realized. The traditional argon ion polishing sample preparation method of the shale sample is to cut a block-shaped sample which is convenient to hold by hand from an original shale sample, bond the sample on a polishing sample table after mechanical polishing on one side, and place the sample in an argon ion polisher for polishing (see the argon ion polisher instrument operation instruction). Coke shu et al (2016) compared with the traditional natural section method and argon ion polishing method, although argon ion polishing method is easier to identify organic matter and suitable for observing organic matter pores, it takes longer time. The embedding method used by wangliang et al (2015) expands the analysis range of samples, improves the success rate of shale core samples which are very easy to break, but only aims at a single sample, and is long in time consumption. Generally, a single sample argon ion polishing step (including mechanical cutting, rough grinding, fine grinding, argon ion polishing and the like) is long in period, generally, a flow usually needs more than 5 hours, and the efficiency is low. Therefore, attention has been paid to how to achieve single batch multi-sample polishing of shale samples to improve polishing efficiency and reduce costs, but previous approaches have not explored this.

In addition, because the surface conductivity of the rock sample is poor, charge aggregation is easily generated under a scanning electron microscope to influence the imaging quality, and particularly, when the content of the carbonate rock is high or the evolution degree of organic matters is low, the charge aggregation effect becomes more remarkable, and a clear image is difficult to obtain. The embedding agent used in the embedding method used in the above-mentioned royal jelly et al (2015) is a non-conductive material, and is not favorable for observation by a scanning electron microscope. The gold spraying method can be adopted for the conventional reservoir stratum to improve the conductivity of the rock surface, but the gold cost is high. Liu Xinnian et al (2013) propose a copper plating method for a rock sample of a scanning electron microscope, utilize metallic copper to replace noble metal gold to carry out film plating, improve the conductivity, but for dense shale, the surface either spraying gold or plating copper can cause gold and copper particles to cover the nanopores, and the polishing effect is influenced. Therefore, it is also highly desirable to consider how to optimize and improve the surface conductivity of the sample so as to achieve high-efficiency and high-quality polishing.

Disclosure of Invention

The invention aims to provide a multi-sample preparation device and method suitable for argon ion polishing, which can be used for preparing a plurality of rock samples at one time, improving the efficiency of subsequent polishing and saving the cost.

To achieve the above object, the present invention provides a multi-sample preparation apparatus suitable for argon ion polishing, comprising:

the base tray is provided with a first through hole;

the top cover is detachably connected to the base tray, and a positioning mechanism is arranged on the top cover;

the sample seat is arranged on the base tray, a plurality of second through holes are formed in the sample seat, the second through holes are used for placing rock samples, and when the top cover is connected to the base tray, the rock samples are fixed in the second through holes through the positioning mechanism;

a reaction vessel capable of receiving the base tray.

Preferably, the first through holes are multiple, and the multiple first through holes are arranged at the bottom of the base tray.

Preferably, the top cover is provided with a plurality of threaded holes penetrating through the top cover, when the top cover is connected to the base tray, each threaded hole corresponds to one of the second through holes, the positioning mechanism comprises a plurality of threaded ejector rods, and each threaded ejector rod is in threaded connection with one of the threaded holes so as to fix the rock sample in the second through hole.

Preferably, the base tray with the top cap passes through threaded connection, just the base tray with the junction of top cap is equipped with the sealing washer.

Preferably, the number of the first through holes is greater than the number of the second through holes; and/or

The first through hole and the second through hole are both cylindrical holes, and the diameter of the first through hole is smaller than that of the second through hole.

Preferably, the bottom surface of the base tray is provided with a polytetrafluoroethylene coating, and/or the reaction vessel is made of polytetrafluoroethylene.

Preferably, the reactor further comprises a heater arranged below the reaction vessel.

Preferably, the material of the sample holder is metal.

A method of preparing multiple samples suitable for argon ion polishing, comprising:

step 1: placing the sample seat on the base tray, selecting a plurality of rock samples, and placing each rock sample in one second through hole to form a gap between the periphery of the rock sample and the inner wall of the second through hole;

step 2: connecting the top cover to the base tray, and fixing the rock sample in the second through hole through the positioning mechanism;

and step 3: placing the base tray in the reaction vessel, pouring molten metal into the reaction vessel and immersing the first through holes in the molten metal;

and 4, step 4: heating molten metal in the reaction vessel;

and 5: stopping heating, and taking out the sample holder after the molten metal is solidified.

Preferably, in the step 4, the heating temperature is higher than the melting point of the metal.

Preferably, in the step 3, the metal is a low melting point alloy.

Preferably, the height of the rock sample is greater than or equal to the depth of the second through hole.

The invention has the beneficial effects that:

1. the preparation device can prepare a plurality of rock samples for argon ion polishing at a time including the sample seat that is provided with a plurality of through-holes to the fixed problem of rock sample has been solved, and follow-up can carry out argon ion polishing simultaneously to a plurality of rock samples in the sample seat, has effectively improved the efficiency of argon ion polishing, is of value to practicing thrift the cost.

2. The sample seat of the preparation device is made of metal, the rock sample and the sample seat are adhered together through molten metal, and the surface conductivity of the rock sample can be remarkably improved by means of the conductivity of the metal sample seat and the metal, so that the accumulation effect of an electron beam on the surface of the rock sample when a scanning electron microscope is used for observing the rock sample polished by argon ions is effectively overcome.

3. The base tray is coated with polytetrafluoroethylene film, so that the formed sample seat is separated from the solidified metal conveniently.

The apparatus and methods of the present invention have other features and advantages which will be apparent from or are set forth in detail in the accompanying drawings and the following detailed description, which are incorporated herein, and which together serve to explain certain principles of the invention.

Drawings

The above and other objects, features and advantages of the present invention will become more apparent by describing in more detail exemplary embodiments thereof with reference to the attached drawings, in which like reference numerals generally represent like parts.

FIG. 1 shows a schematic diagram of a multi-sample preparation device suitable for argon ion polishing according to one embodiment of the present invention.

Figure 2 shows a flow chart of a method of multi-sample preparation suitable for argon ion polishing according to the present invention.

Fig. 3 shows a comparison of a multi-sample preparation prepared according to the preparation method of the present invention and a single-sample preparation prepared according to a conventional preparation method.

Fig. 4a shows the observation effect of the shale sample polished by the conventional argon ions in a scanning electron microscope.

Fig. 4b is a graph showing the observation effect of a shale sample prepared by the multi-sample preparation method suitable for argon ion polishing in a scanning electron microscope according to one embodiment of the invention.

Description of reference numerals:

1. a base tray; 2. a top cover; 3. a sample holder; 4. a reaction vessel; 5. a threaded ejector rod; 6. a first through hole; 7. a second through hole; 8. a heater.

Detailed Description

The invention will be described in more detail below with reference to the accompanying drawings. While the preferred embodiments of the present invention are shown in the drawings, it should be understood that the present invention may be embodied in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.

A multi-sample preparation device suitable for argon ion polishing according to the present invention comprises:

the base tray is provided with a first through hole;

the top cover is detachably connected to the base tray, and a positioning mechanism is arranged on the top cover;

the sample seat is arranged on the base tray, a plurality of second through holes are formed in the sample seat and used for placing rock samples, and when the top cover is connected to the base tray, the rock samples are fixed in the second through holes through the positioning mechanism;

a reaction vessel capable of receiving the base tray.

Specifically, can place a plurality of rock specimen simultaneously through the sample seat that is provided with a plurality of through-holes, can fix the rock specimen in the through-hole of sample seat through stop gear after top cap and base tray are connected, make the bottom and the base tray contact of rock specimen. When a sample is prepared, the base tray is placed in the reaction container, molten metal is poured into the reaction container, the molten metal permeates between the base tray and the sample seat through the first through hole and then enters the second through hole, and the rock samples are fixed in the second through hole after cooling, so that the fixation of a plurality of rock samples is realized, and the subsequent argon ion polishing is facilitated.

In one example, the first through hole is a plurality of through holes, and the plurality of first through holes are arranged at the bottom of the base tray.

Specifically, the bottom of base tray is located to first through-hole, can communicate with the second through-hole of sample seat, is convenient for be used for the molten metal infiltration second through-hole of bonding rock specimen and sample seat and contact with the rock specimen.

In one example, the top cover is provided with a plurality of threaded holes extending through the top cover, each threaded hole corresponding to one of the second through holes when the top cover is attached to the base tray, and the positioning mechanism includes a plurality of threaded push rods, each threaded push rod being threadedly attached within one of the threaded holes to secure the rock sample within the second through hole.

Specifically, the screw ejector rod is arranged along the vertical direction and matched with a vertical screw hole penetrating through the top cover, and when the top cover is connected with the base tray, the screw hole in the top cover corresponds to the position of the second through hole of the sample seat. Can rotate every screw ejector pin respectively to adjust the screw in degree of depth of every screw ejector pin respectively, thereby fix the rock specimen in every second through-hole, prevent that the rock specimen from floating in the molten metal influence to adhere the effect.

In one example, the base tray is connected with the top cover through threads, and a sealing ring is arranged at the joint of the base tray and the top cover.

Specifically, base tray and top cap are the cylinder, and base tray upper portion border and top cap lower part border all are provided with the screw thread, and the connection is realized in the cooperation of the two screw thread, still is provided with the sealing rubber ring in the junction. The material of base tray and top cap all chooses corrosion-resistant stainless steel for use, can suitably increase the weight of top cap in order to increase decurrent pressure to can make the base tray submergence in the molten metal after top cap and base tray are connected.

In one example, the number of first vias is greater than the number of second vias; and/or

The first through hole and the second through hole are both cylindrical holes, and the diameter of the first through hole is smaller than that of the second through hole.

Specifically, first through-hole and second through-hole are the cylindrical through-hole that vertical direction set up, and the diameter of first through-hole should be less than the diameter of second through-hole to make the bottom of rock specimen can push up and can not deviate from first through-hole at the bottom of the base tray, the quantity of first through-hole should be greater than the second through-hole simultaneously, and porous network structure is of value to rock specimen and molten metal and fully contacts.

In one example, the bottom surface of the base tray is provided with a teflon coating, and/or the reaction vessel is made of teflon.

Specifically, the melting point of the polytetrafluoroethylene is 327 degrees, the polytetrafluoroethylene is a high-temperature-resistant release agent, and after the polytetrafluoroethylene is sprayed on the base tray, the base tray is easy to separate from solidified metal after the molten metal is solidified, and the sample holder is also easy to separate from the base tray. The reaction vessel is made of polytetrafluoroethylene to facilitate separation of the solidified molten metal.

In one example, a heater disposed below the reaction vessel is also included.

Specifically, the heater may be a heating table disposed below the reaction vessel to heat the molten metal in the reaction vessel.

In one example, the sample holder is made of metal.

Specifically, the sample holder should be conductive metal, and can select red copper with good conductivity, and the red copper has low cost and excellent conductivity compared with gold and silver.

Figure 2 shows a flow chart of the steps of a method of multi-sample preparation suitable for argon ion polishing according to the present invention.

As shown in fig. 2, a method for preparing multiple samples suitable for argon ion polishing comprises:

step 1: placing the sample seat on a base tray, selecting a plurality of rock samples, and placing each rock sample in one second through hole to form a gap between the periphery of the rock sample and the inner wall of the second through hole;

step 2: connecting the top cover to the base tray, and fixing the rock sample in the second through hole through the positioning mechanism;

and step 3: placing the base tray in a reaction vessel, pouring molten metal into the reaction vessel and immersing the first through holes in the molten metal;

and 4, step 4: heating molten metal in a reaction vessel;

and 5: the heating was stopped and the sample holder was removed after the molten metal solidified.

In one example, in step 4, the heating temperature is above the melting point of the metal.

In one example, in step 3, the metal is a low melting point alloy.

Specifically, the low-melting point alloy refers to a metal having a melting point of 300 ℃ or lower and an alloy thereof, and is usually composed of low-melting point metal elements such as Bi, Sn, Pb, and In. These alloys are commonly used to make plastic, drawing and forming dies. Utilize the low characteristics of low melting point alloy melting point can be comparatively easy to make it become liquid through the heating, make the molten alloy fully fill the space between rock specimen and the second through-hole through continuously heating in the settlement time, after cooling to room temperature low melting point alloy solidification after stopping heating, rock specimen and sample holder can adhere together, realize the fixed of many samples, are convenient for once only carry out argon ion polishing to a plurality of rock specimens, effectively improve polishing efficiency. In addition, the low melting point alloy of gluing can increase the electric conductivity between rock specimen surface and the metal sample seat, and the sample seat that the preparation was accomplished is directly arranged in scanning electron microscope equipment and is observed, and alloy and metal sample seat all have better electric conductivity, can overcome the accumulative effect of electron beam on rock specimen surface when scanning electron microscope observes, the imaging quality when the follow-up scanning electron microscope of effectual improvement is observed.

In one example, the height of the rock sample is greater than or equal to the depth of the second through hole.

Specifically, the selected rock sample can be a columnar rock sample with the diameter smaller than that of the second through hole, the upper end of the rock sample is a plane subjected to coarse grinding and fine grinding, and the rock sample is placed in the second through hole to form a gap with the inner wall of the second through hole so that molten metal can permeate into the gap conveniently. The height of the rock sample is preferably not less than the depth of the second through hole, so that the problem that the upper end of the rock sample is recessed into the through hole and cannot be polished or polished due to subsequent argon ion polishing is solved.