阅读说明：本技术 一种离子探针样品靶及其制备方法 (Ion probe sample target and preparation method thereof ) 是由 李娇 马红霞 李秋立 于 2020-05-26 设计创作，主要内容包括：本发明提供一种离子探针样品靶及其制备方法,涉及离子探针技术领域,上述离子探针样品靶包括：待测样品靶和标准物质小靶；待测样品靶上设置有标准物质槽；标准物质小靶嵌装在标准物质槽内,并与待测样品靶表面相平。该离子探针样品靶在测试后可将其中的标准物质小靶卸取下来,抛磨掉表面的测试坑后再次与其他样品组合制备进行测试,可使得离子探针标准物质多次循环使用,缓解离子探针标准物质日渐匮乏的现状。(The invention provides an ion probe sample target and a preparation method thereof, relating to the technical field of ion probes, wherein the ion probe sample target comprises the following components: a sample target to be detected and a small standard substance target; a standard substance groove is arranged on the sample target to be detected; the small standard substance target is embedded in the standard substance groove and is level with the surface of the sample target to be measured. The ion probe sample target can be used for detaching the small target of the standard substance after testing, and is combined with other samples for preparation and testing after a test pit on the surface is polished off, so that the ion probe standard substance can be recycled for many times, and the current situation that the ion probe standard substance is deficient day by day is relieved.)

1. An ion probe sample target, comprising: a sample target to be detected and a small standard substance target;

a standard substance groove is formed in the sample target to be detected;

the small standard substance target is embedded in the standard substance groove and is level to the surface of the sample target to be detected.

2. The sample target of claim 1, wherein at least one sample to be tested is on the sample target to be tested.

3. The sample target according to claim 1, wherein the distance of the standard substance in the small target of standard substance is not less than 0.5mm from the edge.

4. The sample target according to claim 1, wherein the sample target material is metallic indium or resin;

preferably, when the sample target is made of indium metal, the sample target to be detected comprises a small sample target to be detected and an indium matrix, and the small sample target to be detected is embedded on the indium matrix.

5. The method for preparing a sample target according to any one of claims 1 to 4, wherein when the material of the sample target is indium metal, the method comprises the steps of:

respectively sticking a standard substance and a sample to be detected on the double-sided adhesive of the two glass plates;

blending resins and respectively infusing, and after the resins are cured, respectively polishing until the standard substance and the sample to be detected are exposed on the surface;

drilling a standard substance infused with resin and a sample to be detected to respectively obtain a small target of the standard substance and a small target of the sample to be detected;

flatly pressing metal indium into a target holder to obtain an indium matrix, and drilling a sample groove and a standard substance groove on the surface of the indium matrix;

and correspondingly pressing the small target of the sample to be detected and the small target of the standard substance into the sample groove and the standard substance groove to obtain the sample target.

6. The method according to claim 5, wherein a closest distance between any two of the sample well and the standard substance well is at least 2 mm.

7. The method of manufacturing according to claim 5, further comprising:

and polishing the side surfaces of the drilled small standard substance target and the small sample target to be detected.

8. The method for preparing a sample target according to any one of claims 1 to 4, wherein when the sample target is made of a resin, the method comprises the steps of:

respectively sticking a standard substance and a sample to be detected on the double-sided adhesive of the two glass plates;

blending resins and respectively infusing, and after the resins are solidified, respectively polishing until the standard substance and the sample to be detected are exposed on the surface to obtain a standard substance target and a sample target to be detected;

drilling a standard substance on the standard substance target to obtain a small standard substance target;

drilling a standard substance groove at a blank position above a sample target to be detected;

and pressing the small standard substance target into the standard substance groove to obtain the sample target.

9. The method of claim 8, wherein the step of pressing the small target of standard substance into the standard substance groove comprises:

firstly, adding a proper amount of metal indium into a standard substance groove, and then pressing a small standard substance target into the standard substance groove.

10. The method according to claim 9, wherein the standard substance groove has a pore diameter 0.8 to 1.5mm larger than the diameter of the standard substance small target; the depth of the standard substance groove is 0.2-0.5 mm greater than the thickness of the standard substance small target.

Technical Field

The invention relates to the technical field of ion probes, in particular to an ion probe sample target and a preparation method thereof.

Background

The ion probe (SIMS) has the advantages of high mass resolution, high sensitivity and high analysis precision, small analysis beam spot (generally less than 20 microns), and low sample consumption (10)^-9Gram) has irreplaceable technical advantages in the field of micro-area in-situ analysis, and is widely applied to the fields of geoscience, celestial geology and environmental geology.

The ion probe analysis technology mainly comprises two important links of sample preparation and instrument test analysis, and the preparation of an applicable sample target is an important basis for obtaining reliable data. At present, ion probe laboratories inside and outside China have very mature methods for preparing and testing solid samples. The ion probe sample target is limited by various conditions such as the states of an instrument sample clamp and a sample bin, and is usually adhered to a smooth and clean glass plate cleaned by alcohol by adopting a double-sided adhesive tape (3M brand and the like) with uniform thickness, 4-5 pieces of sample particles and corresponding standard substance particles are respectively adhered, and a sample target diagram is carefully drawn so as to be distinguished at a later stage; then blending resin according to the proportion, adopting a one-inch grinding tool to place the sample and the standard substance within 1.5 cm of the circle center, pouring the resin, and polishing after curing; or pressing the sample and the standard substance particles into a flat indium sample groove by using an indium target flattening instrument, for example, taking zircon as an example, as shown in fig. 1, 4 different samples can be stuck on one sample target, and each sample is stuck in a row of about 200 samples; at present, an ion probe has a very mature zircon dating, oxygen, lithium isotope and other isotope determination method, at least three standard substances are required to be pasted when a zircon mineral sample target is prepared, and a main zircon dating standard substance Plesovice, an oxygen isotope standard substance Penglai and at least one 'blind mark' Qinghu are taken as unknown samples to be corrected; and after the adhesion is finished, epoxy resin is poured, the surface of the sample is polished to be flat after the solidification, the sample target is in a one-inch cylinder shape, the overall thickness is about 5 millimeters, the requirement of an instrument sample Holder is met, and then the sample can be cleaned, plated with gold and then put on a machine for testing.

In the process of generating secondary ions by primary ion bombardment of the ion probe, the difference of ionization efficiency among different elements can reach several orders of magnitude, even if the yields of nuclides of the same element with different mass numbers are different, the nuclides are changed along with the difference of sample components and structures, namely the matrix effect. Therefore, standard substances of the same composition and structure as the unknown sample are required to correct the fractionation; in order to correctly detect the fractionation effect, the standard substance and the unknown sample need to be pasted on the same sample target for detection under the same instrument condition; meanwhile, in order to detect the correctness of analysis, another standard substance or a plurality of standard substances are required to be simultaneously prepared as unknown samples for analysis, so that 2 to 3 standard substances are required on one sample target at the same time, and each sample has dozens of particles; since the standard substance has a very small particle size (about 100 μm), is buried in resin and is difficult to take out, the standard substance cannot be recycled after detection, and the standard substance has a long development period and a high difficulty, so that the shortage of the standard substance inevitably becomes one of the most important problems in laboratories.

Disclosure of Invention

In view of the above, the present invention is directed to an ion probe sample target and a method for preparing the same, in which a standard substance in the ion probe sample target can be recovered for reuse, thereby solving the problem that the standard substance cannot be recycled.

In view of the above object, the present invention provides in a first aspect an ion probe sample target comprising: a sample target to be detected and a small standard substance target;

a standard substance groove is formed in the sample target to be detected;

the small standard substance target is embedded in the standard substance groove and is level to the surface of the sample target to be detected.

Preferably, at least one sample to be tested is arranged on the sample target to be tested.

Preferably, the small target of the standard substance is positioned in the middle of the target of the sample to be detected.

Preferably, the thickness of the sample target to be detected is 4-6 mm, and the thickness of the small standard substance target is 2-3 mm.

Preferably, the distance between the standard substance in the small standard substance target and the edge is not less than 0.5 mm; more preferably, the small standard substance target is cylindrical and has a diameter of 3-4 mm.

Preferably, the sample target material is metallic indium or resin.

Preferably, when the material of the sample target is metal indium, the sample target to be detected comprises a small sample target to be detected and an indium matrix, and the small sample target to be detected is embedded on the indium matrix;

before the sample target is detected by the machine, the sample target is cleaned, dried and plated with gold by adopting high-purity water and alcohol.

In a second aspect of the present invention, when the sample target is made of indium, the method for preparing the sample target includes the following steps:

respectively sticking a standard substance and a sample to be detected on the double-sided adhesive of the two glass plates;

blending resins and respectively infusing, and after the resins are cured, respectively polishing until the standard substance and the sample to be detected are exposed on the surface;

drilling a standard substance infused with resin and a sample to be detected to respectively obtain a small target of the standard substance and a small target of the sample to be detected;

flatly pressing metal indium into a target holder to obtain an indium matrix, and drilling a sample groove and a standard substance groove on the surface of the indium matrix;

and correspondingly pressing the small target of the sample to be detected and the small target of the standard substance into the sample groove and the standard substance groove to obtain the sample target.

Preferably, a plurality of samples to be detected are pasted on the double-sided adhesive of the glass plate, and the pasting range of each sample to be detected is 4-5 mm; more preferably, the number of the adhered particles of each sample to be detected is 150-200; more preferably, the wiping is performed with alcohol-stained dust-free paper before the double-sided tape is fixed on the glass plate.

Preferably, the preparation method further comprises:

before the small standard substance target and the small sample target to be detected are pressed into the sample groove and the standard substance groove, the side surfaces of the drilled small standard substance target and the drilled small sample target to be detected are polished.

Preferably, the step of pressing the indium metal flatly into the target holder specifically comprises:

placing metal indium in a groove in the center of the target holder, and heating to melt the metal indium; and then, cooling to 95-105 ℃, placing the target holder in a flattening instrument, and flattening the metal indium until the surface is flat.

Preferably, the closest distance between any two of the sample and standard wells is at least 2 mm.

Preferably, the sample groove is the same as the small target of the sample to be detected, and the standard substance groove is the same as the small target of the standard substance.

The third aspect of the present invention provides a method for preparing the sample target, where the material of the sample target is resin, the method comprising the following steps:

respectively sticking a standard substance and a sample to be detected on the double-sided adhesive of the two glass plates;

blending resins and respectively infusing, and after the resins are solidified, respectively polishing until the standard substance and the sample to be detected are exposed on the surface to obtain a standard substance target and a sample target to be detected;

drilling a standard substance on the standard substance target to obtain a small standard substance target;

drilling a standard substance groove at a blank position above a sample target to be detected;

and pressing the small standard substance target into the standard substance groove to obtain the sample target.

Preferably, a plurality of samples to be detected are pasted on the double-sided adhesive of the glass plate, and the pasting range of each sample to be detected is 4-5 mm; more preferably, the number of the adhered particles of each sample to be detected is 150-200; more preferably, the wiping is performed with alcohol-stained dust-free paper before the double-sided tape is fixed on the glass plate.

Preferably, the process of pressing the small standard substance target into the standard substance groove comprises:

firstly, adding a proper amount of metal indium into a standard substance groove, and then pressing a small standard substance target into the standard substance groove.

Preferably, the aperture of the standard substance groove is 0.8-1.5 mm larger than the diameter of the standard substance small target; the depth of the standard substance groove is 0.2-0.5 mm greater than the thickness of the standard substance small target.

As can be seen from the above description, the ion probe sample target and the preparation method thereof provided by the present invention at least have the following beneficial effects:

the preparation method of the ion probe sample target is easy to operate, can be popularized and used in a large range, is not easy to cause the sample to be polluted in the preparation process, and can ensure the surface flatness and the bonding fastness of the small standard substance target and the sample target to be detected so as to ensure the accuracy of the detection result; in addition, the ion probe sample target prepared by the preparation method can be taken down after being tested, and is combined with other samples again for testing after a test pit on the surface is polished off, so that the ion probe standard substance can be recycled for multiple times, and the current situation that the ion probe standard substance is deficient day by day is relieved.

Drawings

In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.

FIG. 1 is a schematic diagram of a prior art ion probe sample target provided in the background of the invention;

FIG. 2 is a schematic diagram of an exploded structure of a resin target of an ion probe sample according to an embodiment of the present invention;

fig. 3 is a schematic diagram of an explosion structure of an indium target of an ion probe sample according to an embodiment of the present invention.

Shown in the figure:

1-sample target to be detected, 11-small sample target to be detected, 12-indium matrix, 13-standard substance groove and 14-sample groove; 2-Small target of Standard substance.

Detailed Description

In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to specific embodiments and the accompanying drawings.

It is to be noted that technical terms or scientific terms used in the embodiments of the present invention should have the ordinary meanings as understood by those having ordinary skill in the art to which the present disclosure belongs, unless otherwise defined. The use of the word "comprising" or "comprises", and the like, in this disclosure is intended to mean that the elements or items listed before that word, include the elements or items listed after that word, and their equivalents, without excluding other elements or items.

There is a very significant "matrix effect" during ion probe (SIMS) sample analysis; due to the limitation of various factors such as instrument design and the influence of sample surface smoothness on a test result, the standard substance and a sample to be tested are prepared on one sample target for analysis; after the test is finished, the standard substance has extremely small particle size (about 100 micrometers) and is buried in resin, so that the standard substance is difficult to take out and cannot be reused for multiple times.

In view of the above, embodiments of the present invention provide an ion probe sample target, as shown in fig. 2 and 3, the ion probe sample target includes: a sample target 1 to be detected and a small standard substance target 2;

a standard substance groove 13 is arranged on the sample target 1 to be detected;

the small standard substance target 2 is embedded in the standard substance groove 13 and is level with the surface of the sample target 1 to be measured.

According to the invention, the standard substance and the sample target 1 to be detected can be divided into two detachable parts by the arrangement of the small standard substance target 2, and after the detection of the sample to be detected is finished, the small standard substance target 2 can be taken out from the sample target 1 to be detected and then assembled for repeated use, so that the current situation that the standard substance of the ion probe is gradually deficient is relieved.

The invention does not strictly limit the taking-out mode of the small standard substance target 2, for example, the small standard substance target 2 can be taken out by cutting, or the small standard substance target 2 can be taken out by using tweezers after heating; preferably, the small target 2 of the standard substance is taken out by cutting.

In the ion probe detection process, the number of samples to be detected on the sample target 1 to be detected can be reasonably selected according to actual needs, for example, in one embodiment, there is one sample to be detected on the sample target 1 to be detected; in other embodiments, 3, 4, or 5; through the setting of a plurality of samples that await measuring, can detect a plurality of samples that await measuring simultaneously, improve detection efficiency.

In order to improve the accuracy of the detection, in some embodiments, the small target 2 of the standard substance is located in the middle of the target of the sample to be detected.

The thickness of the sample target 1 to be detected and the thickness of the small standard substance target 2 are not strictly limited, and preferably, the thickness of the small standard substance target 2 is not more than the thickness of the sample target 1 to be detected; for example, the thickness of the sample target 1 to be measured can be 4-6 mm, and the thickness of the small standard substance target 2 can be 2-3 mm; in one embodiment, the thickness of the sample target 1 to be measured may be 5mm, and the thickness of the small target 2 of the standard substance may be 3 mm.

In one embodiment, the distance of the standard substance in the small standard substance target 2 from the edge is not less than 0.5 mm; through the injecing of standard substance apart from the distance of edge, can ensure 2 inlays adorn the in-process at standard substance small target, prevent that standard substance from receiving the extrusion of edge, influencing the testing result.

In one embodiment, the small target 2 of the standard substance is cylindrical and has a diameter of 3 to 4 mm.

The material of the sample target is not limited strictly, and may be selected according to actual needs, for example, the material of the sample target may be metal indium or resin.

In one embodiment, when the sample target is made of indium metal, as shown in fig. 3, the sample target 1 to be measured includes a small sample target 11 to be measured and an indium substrate 12, and the indium substrate 12 is provided with a standard substance groove 13 and a sample groove 14; the sample small target 11 to be measured is embedded in the sample groove 14.

The embodiment of the invention also provides a preparation method of the ion probe sample indium target, which comprises the following steps:

respectively sticking a standard substance and a sample to be detected on the double-sided adhesive of the two glass plates;

blending resins and respectively infusing, and after the resins are cured, respectively polishing until the standard substance and the sample to be detected are exposed on the surface;

drilling a standard substance infused with resin and a sample to be detected to respectively obtain a small target 2 of the standard substance and a small target 11 of the sample to be detected;

flatly pressing metal indium into a target holder to obtain an indium substrate 12, and drilling a sample groove 14 and a standard substance groove 13 on the surface of the indium substrate 12;

and correspondingly pressing the small target 11 of the sample to be detected and the small target 2 of the standard substance into the sample groove 14 and the standard substance groove 13 to obtain the indium target of the ion probe sample.

The preparation method is easy to operate, can be popularized and used in a large range, is not easy to cause the sample to be polluted in the preparation process, and can ensure the surface flatness and the bonding fastness of the small standard substance target 2 and the sample target 1 to be detected so as to ensure the accuracy of the detection result.

In one embodiment, before the double-sided adhesive tape is fixed on the glass plate, the double-sided adhesive tape is wiped by using dust-free paper stained with alcohol, and the surface of the stuck double-sided adhesive tape is flat and free from bubbles; the method is beneficial to improving the smoothness of the sample to be detected and the standard substance, and avoids the existence of impurities to influence the detection accuracy.

Further, adhering a plurality of samples to be detected on the double-sided adhesive of the glass plate, wherein the adhering range of each sample to be detected is 4-5 mm, and specifically, each sample to be detected is adhered in a circular range with the diameter range of 4mm or 5 mm; the number of the adhered particles of each sample to be detected is 150-200, and specifically 150, 180 or 200. Through pasting of a plurality of samples that await measuring, can realize detecting a plurality of samples simultaneously, improve detection efficiency.

The above-mentioned preparation method of the present invention does not strictly limit the distribution of the sample well and the standard substance well, and for example, in one embodiment, the closest distance between any two wells of the sample well 14 and the standard substance well 13 is at least 2 mm; in particular, it may be 2mm, 3mm or 4 mm. Through the limitation of the nearest distance between any two grooves, the indium metal between the grooves is prevented from deforming or cracking to affect the flatness of the surface when the small target of the sample to be detected and the small target of the standard substance are pressed into the corresponding grooves.

In one embodiment, the sample groove 14 is the same size as the small target 11 of the sample to be measured, and the standard substance groove 13 is the same size as the small target 2 of the standard substance; the small target of the sample to be detected and the small target of the standard substance are tightly combined with the indium matrix, and the stability is improved.

In one embodiment, the above preparation method further comprises:

before the small standard substance target 2 and the small sample target 11 to be detected are pressed into the sample groove 14 and the standard substance groove 13, the side surfaces of the drilled small standard substance target 2 and the drilled small sample target 11 to be detected are polished. The small target 2 of the standard substance and the small target 11 of the sample to be detected are favorably and tightly combined with the corresponding sample groove 14 and the standard substance groove 13, so that the generation of air gaps is prevented, and the connection stability and the surface flatness of the small target 2 of the standard substance and the small target 11 of the sample to be detected on the indium substrate 12 are improved.

The manner in which the indium metal is flatly pressed into the backing plate is not critical and can be conventional in the art, for example, in one embodiment, the indium metal is placed in a groove in the center of the backing plate and heated to melt; and then, cooling to 95-105 ℃, placing the target holder in a flattening instrument, and flattening the metal indium until the surface is flat.

Further, the target holder is a non-magnetic stainless steel target holder, and the conventional target holder in the field can be adopted. The selection of the non-magnetic stainless steel target holder does not influence the magnetic field of the ion probe.

The embodiment of the invention also provides a preparation method of the ion probe sample resin target, which comprises the following steps:

respectively sticking a standard substance and a sample to be detected on the double-sided adhesive of the two glass plates;

blending resins and respectively infusing, and after the resins are solidified, respectively polishing until the standard substance and the sample to be detected are exposed on the surface to obtain a standard substance target and a sample target 1 to be detected;

drilling a standard substance on the standard substance target to obtain a small standard substance target 2;

drilling a standard substance groove 13 at the blank position above a sample target 1 to be detected;

and pressing the small standard substance target 2 into the standard substance groove 13 to obtain the ion probe sample resin target.

In one embodiment, a plurality of samples to be tested are pasted on the double-sided adhesive of the glass plate, for example, 1, 3, 4 or 5 samples can be pasted; the sticking range of each sample to be detected is 4-5 mm, and specifically can be in a circular area with the diameter of 4mm or a circular area with the diameter of 5 mm; the number of the adhered particles of each sample to be detected is 150-200; through pasting of a plurality of samples that await measuring, can realize detecting a plurality of samples simultaneously, improve detection efficiency.

Further, before the double-sided adhesive tape is fixed on the glass plate, the double-sided adhesive tape is wiped by using dust-free paper stained with alcohol, and the double-sided adhesive tape is flat and free of bubbles.

In one embodiment, the step of pressing the small standard substance target 2 into the standard substance groove 13 includes adding an appropriate amount of indium metal into the standard substance groove 13 and then pressing the small standard substance target 2 into the standard substance groove 13.

Further, the aperture of the standard substance groove 13 is 0.8-1.5 mm larger than the diameter of the standard substance small target 2, specifically 0.8mm, 1mm or 1.5 mm; the depth of the standard substance groove 13 is 0.2-0.5 mm larger than the thickness of the standard substance small target, specifically 0.2mm, 0.3mm or 0.5 mm.

In the pressing-in process, a proper amount of metal indium is added, so that the metal indium can be filled between the small standard substance target 2 and the standard substance groove 13, the generation of a gap is avoided, and the stability and the surface flatness of the small standard substance target 2 on the sample target 1 to be detected are improved.

The overall technical solution of the present invention will be further described in detail by specific examples.