CN107449648A - A kind of preparation method of the sample target of ore mineral suitable for ion microprobe analysis - Google Patents
A kind of preparation method of the sample target of ore mineral suitable for ion microprobe analysis Download PDFInfo
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- CN107449648A CN107449648A CN201710520161.7A CN201710520161A CN107449648A CN 107449648 A CN107449648 A CN 107449648A CN 201710520161 A CN201710520161 A CN 201710520161A CN 107449648 A CN107449648 A CN 107449648A
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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
- G01N1/32—Polishing; Etching
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
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Abstract
The invention discloses a kind of preparation method of the sample target of the ore mineral suitable for ion microprobe analysis, epoxy resin instead of using alloy material, target material hardness processed is moderate, it is adapted to grinding and buffing, it can effectively solve the problem that epoxy resin " outgassing ", indium target in high vacuum environment are difficult to suppress to little particle Within Monominerals, it is difficult to the problems such as carrying out sanding and polishing.
Description
Technical field：
The present invention relates to geological sample detection technique field, and in particular to a kind of to be applied to what ion microprobe was analyzed
The preparation method of the sample target of ore mineral.
Background technology：
Ore mineral individual particle is very small, such as zircon, and its granular size is generally 200 mesh or so, carry out it is secondary from
When sub- mass spectrograph (SIMS) analysis, individual particle operation can not be carried out, therefore be required to sample carrying out target processed.Sample target is circle
Cylindricality, its basal diameter are 1 inch (25.4mm), and according to the optimum position of ion stream when testing, ore mineral is placed on into sample
On position at product pinwheel 8-15mm.When carrying out sims analysis, sample target is put into the sample carrier of instrument, utilizes sample
Sample target is fixed in sample carrier by circular ring plate wide support edge 3mm and the baffle plate at the back side.Conventional method is to glue list at present
Epoxy resin is poured in the mould of mineral, polishing is removed after complete cooling condenses, obtains a plane at ore mineral center,
Finally carry out dependence test.The target production technique is low with cost, and technique is simpler, and sample target high mechanical strength, shrinkage factor is low,
Stable performance, there is the advantages such as good cementitiousness, be most widely used sample target preparation method.But because of asphalt mixtures modified by epoxy resin
Fat belongs to highly polar resin, has stronger compatibility to hydrone, has certain water absorption rate, be typical absorbent material.
Though its water absorbing capacity of different epoxy resin is also not quite similar, its water absorption rate of some products can reach 2.0%, even more high.Cause
, when sample target is placed in vacuum environment, hydrone easily breaks away from the constraint of epoxy resin, is gradually released into sample cavity for this.Institute
In good fortune overwhelming majority application, such as the U-Pb of zircon determines year, trace element analysis, pyritic sulfur isotope analysis etc., asphalt mixtures modified by epoxy resin
Destruction of the fat " outgassing " on vacuum is not enough to influence the analysis result of above element, therefore does not draw attention.
If the element analyzed (such as oxygen isotope, if epoxy resin strong " outgassing " will higher to vacuum level requirements
Experiment can be forced to stop), sample target is put in vacuum storage compartment " outgassing " for a long time before need to being analyzed, and carrying out Special Elements
During element analysis, when isotopic content particularly related to H or O-H is analyzed (such as16O1H、1The elements such as H), or to vacuum
When degree requires higher elementary analysis, water equimolecular that epoxy resin is discharged under vacuum conditions, it will improve background value, pole
Big to influence test result, this, which is also forced, changes traditional target production technique.In order to solve this problem, at present more common method be by
Ore mineral has first been polished test surfaces, and is pressed into indium surface, is fabricated to 1 inch of sample target.And this method is in mineral pressure
After entering, the operation such as sanding and polishing can not be carried out, it is therefore desirable to mineral are polished in advance, and indium is pressed into according to certain orientation
In.And for the very tiny Within Monominerals of granularity, the operation such as be difficult to polish in advance, polish.
For very tiny monomineralic of granularity16O1H、1During the analysis of the elements such as H, epoxy resin " outgassing "
Extreme influence data validity, and during use pressure indium target, little particle Within Monominerals are located before being difficult to compacting, grinding and buffing etc.
Reason.Therefore urgently exploitation one kind is used for the monomineralic target production technique of little particle, and it is easy to pouring molding, sanding and polishing, makes simple ore
Thing exposes smooth test plane, without the sample target Target process of contaminated samples, influence sample cavity vacuum.
The content of the invention：
It is an object of the invention to provide a kind of system of the sample target of the ore mineral suitable for ion microprobe analysis
Preparation Method, epoxy resin instead of using alloy material, while target material hardness processed is moderate, is adapted to sanding and polishing, can be effective
Solve epoxy resin " outgassing ", indium target in high vacuum environment little particle Within Monominerals are difficult to suppress, it is difficult to carry out sanding and polishing
The problems such as.
The present invention is achieved by the following technical programs：
A kind of preparation method of the sample target of ore mineral suitable for ion microprobe analysis, including following step
Suddenly：
1) ore mineral sample is fixed on line by line in a diameter of 8-15mm of glass core circle, by a diameter of 20-
30mm mould is fixed to glass core, and mould is concentric with sample；
2) hardness is placed in heating melting in vacuum drying oven in 50-250 DEG C of alloy material in 7-25HBW, fusing point, waits to close
After the melting completely of golden material, the glass plate for being placed with sample and mould that step 1) is obtained is transferred in same vacuum drying oven in advance
Hot 5-10 minutes, molten alloy material is poured into mould, vacuumized, heated, temperature is maintained at the melting temperature of alloy material
On 5-10 DEG C of degree, in vacuum environment after constant temperature 0.5-1 hours, stop vacuumizing, open vent valve, vacuum drying oven is in normal pressure
State, continue constant temperature 0.5-1 hours, after being slowly cooled to room temperature in vacuum tank, take out glass plate, remove mould, taking-up is poured
The sample target built, sanding and polishing is carried out to sample surfaces sample target is made, instrument can be loaded after cleaning and carries out sample test.
Before pouring, the glass plate for being placed with sample and mould is put in the vacuum drying oven of heating molten alloy material and carried out
Preheating, in case rapid condensation-crystallization separates out alloy material to the cold.
Vacuum drying oven needs to deflate before slow cooling is carried out, temperature still need to be maintained at alloy material melting temperature it
On, after certain time, slow cooling pattern can be opened.
Preferably, the alloy material is Babbitt alloy material, tin-dominant, cadmium, bismuth, lead and other elements.
It is single that the ore mineral includes zircon, olivine, apatite, quartz, pyrite, rutile, magnetic iron ore, cassiterite etc.
Mineral.
Beneficial effects of the present invention are as follows：
1) alloy material of the present invention is extremely low in normal temperature and pressure water absorption rate, can effectively avoid epoxy resin in superelevation
In vacuum environment the problem of " outgassing ".
2) when being poured using the alloy material and use the inventive method of the present invention, mineral and the seamless rank of alloy material
Connect, made sample target hardness is moderate, and the operation such as can be polished, polished, and it is difficult effectively to solve pressure indium target small particles Within Monominerals
The problems such as with compacting, grinding and buffing.
In a word, the present invention instead of epoxy resin using alloy material, can effectively avoid epoxy resin in high vacuum ring
In border the problem of " outgassing "；And target material hardness processed is moderate, it is adapted to sanding and polishing；It can effectively solve the problem that indium target to little particle simple ore
Thing is difficult to suppress, it is difficult to the problems such as carrying out sanding and polishing.
Brief description of the drawings：
Fig. 1 is the sample target overall structure diagram obtained after the present invention is poured using alloy material 1；
Fig. 2 is sample part sample distribution figure after the present invention is polished using alloy material 1.
Fig. 3 is the sample target overall structure diagram obtained after the present invention is poured using alloy material 5；
Fig. 4 is sample part sample distribution figure after the present invention is polished using alloy material 5.
Embodiment：
It is to further explanation of the invention, rather than limitation of the present invention below.
Hardness test of the embodiment to alloy material is to use Wilson BH3000A type electricity Zi Bushi Durometer measurements formulas
The hardness of sample cross section, wherein sintered carbide ball a diameter of 5mm, load 62.5kg, keep 30s after press-in, and 5 in embodiment
Shown in kind alloy material design parameter table 1.
The related physicochemical property of 15 kinds of alloy materials of table
| Main component | Solidus (DEG C) | Hardness (HBW) | |
| Alloy material 1 | Tin, lead, bismuth | 70 | 7.92 |
| Alloy material 2 | Tin, bismuth | 138 | 17.51 |
| Alloy material 3 | Bismuth, cadmium, lead | 50 | 9.11 |
| Alloy material 4 | Bismuth, cadmium, lead | 80 | 10.66 |
| Alloy material 5 | Bismuth, cadmium | 90 | 10.17 |
Embodiment 1：
In the present embodiment, zircon standard specimen is selected：Qinghu, Penglai and Plesovices are used as target sample processed, and selection makes
Whole whole target surface after making is illustrated by the use of the Babbitt alloy material 1 in table 1 as material, Fig. 1 is poured.Can from Fig. 2
After going out sanding and polishing, a very smooth zircon particle plane can be obtained.
Concrete operation step is as follows：
Within the scope of the circle for a diameter of 10mm that sticking double faced adhesive tape is drawn a circle to approve on a glass, zircon standard specimen is kept flat line by line viscous
As on double faced adhesive tape, and relative position is recorded.After the completion for the treatment of that sample is placed, the PVC that internal diameter is 25mm is poured into mould
Glass core is sticked to, makes mould concentric with sample, is gently compacted, makes to be seamlessly connected between mould and double faced adhesive tape.Cut about 30g
Babbitt alloy material 1, is placed in Heating Cup, is put in vacuum drying oven and heats melting, after alloy material completely melting, will place
The glass plate of sample and mould is transferred in same vacuum drying oven and preheated 5 minutes, and molten alloy material is poured into mould,
Open vavuum pump to vacuumize, heating in vacuum, temperature is maintained on 10 DEG C of the melting temperature of alloy material, constant temperature in vacuum environment
After 0.5 hour, vavuum pump is closed, opens vent valve, vacuum tank is in atmospheric pressure state, continues heated constant temperature after 0.5 hour, opens
Dynamic slow cooling program, when being slowly cooled to room temperature in vacuum tank, glass plate is taken out, and mould is removed from glass plate,
Take out the metal sample target poured.Whether observation sample target successfully pours, and otherwise needs raising alloy material melt, pour, very
Sky is stood and the time of slow cooling cooling.Most at last sample target polishing, polish and clean after, can examination with computer.Experiment knot
Fruit shows, is put into when by resin target in sample cavity, it is found that vacuum reduces by 1 order of magnitude in sample cavity, over time,
Also setting-out product initial vacuum level can not be evacuated to, and is put into the sample target of new method preparation, sample cavity vacuum has almost no change.
Embodiment 2：
In the present embodiment, zircon standard specimen is selected：Qinghu, Penglai, Plesovices, ZG1, ZG2, ZG3, ZG4 and
ZG5 is used as target sample processed, selects using Babbitt alloy material 5 in table 2 as pouring material, after Fig. 3 illustrates whole making
Whole target surface.As can be seen from Figure 4 after sanding and polishing, a very smooth zircon particle plane can be obtained.
Concrete operation step is as follows：
Within the scope of the circle for a diameter of 10mm that sticking double faced adhesive tape is drawn a circle to approve on a glass, zircon standard specimen is kept flat line by line viscous
Recorded as on double faced adhesive tape and to relative position.After the completion for the treatment of that sample is placed, the PVC that internal diameter is 25mm is poured into mould and glued
To glass core, make mould concentric with sample, be gently compacted, make to be seamlessly connected between mould and double faced adhesive tape.Cut about 30g bars
Family name's alloy material 5, is placed in Heating Cup, is put in vacuum drying oven and heats melting, after alloy material completely melting, will place sample
The glass plate of product and mould is transferred in same vacuum drying oven and preheated 5 minutes, and molten alloy material is poured into mould,
Open vavuum pump to vacuumize, heating in vacuum, temperature is maintained on 10 DEG C of the melting temperature of alloy material, constant temperature in vacuum environment
After 0.5 hour, vavuum pump is closed, opens vent valve, vacuum tank is in atmospheric pressure state, continues heated constant temperature after 0.5 hour, opens
Dynamic slow cooling program, when being slowly cooled to room temperature in vacuum tank, glass plate is taken out, and mould is removed from glass plate,
Take out the metal sample target poured.Observation sample target successfully pours.After sample target is polished, polishes and cleaned, drying is placed in
Stored in case.
Embodiment 3：
Reference implementation example 1, difference are selecting any in table 2 in Babbitt alloy material 2-4 in Babbitt alloy material
Kind.
Claims (3)
- A kind of 1. preparation method of the sample target of ore mineral suitable for ion microprobe analysis, it is characterised in that bag Include following steps：1) ore mineral sample is fixed on line by line in a diameter of 8-15mm of glass core circle, by a diameter of 20-30mm's Mould is fixed to glass core, and mould is concentric with sample；2) hardness is placed in heating melting in vacuum drying oven in 50-250 DEG C of alloy material in 7-25HBW, fusing point, treats alloy material After material melting completely, the glass plate for being placed with sample and mould that step 1) is obtained, which is transferred in same vacuum drying oven, preheats 5- 10 minutes, molten alloy material is poured into mould, vacuumized, heated, temperature is maintained at the melting temperature 5- of alloy material On 10 DEG C, in vacuum environment after constant temperature 0.5-1 hours, stopping vacuumizing, open vent valve, vacuum drying oven is in normal pressure, after Continuous constant temperature 0.5-1 hours, after being slowly cooled to room temperature in vacuum tank, glass plate is taken out, mould is removed, takes out the sample poured Target, sanding and polishing is carried out to sample surfaces sample target is made.
- 2. the preparation method of the sample target of the ore mineral according to claim 1 for ion microprobe analysis, Characterized in that, the ore mineral is Within Monominerals；Its main component of the alloy material is tin, cadmium, bismuth, lead.
- 3. the preparation method of the sample target of the ore mineral according to claim 2 for ion microprobe analysis, Characterized in that, the Within Monominerals include zircon, olivine, apatite, quartz, pyrite, rutile, magnetic iron ore, cassiterite.
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| CN107449648B CN107449648B (en) | 2019-09-27 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108375497A (en) * | 2018-01-23 | 2018-08-07 | 中国科学院地质与地球物理研究所 | A kind of preparation method of secondary ion probe sample target |
| CN111141811A (en) * | 2019-12-26 | 2020-05-12 | 中国科学院地质与地球物理研究所 | Target holder assembly of ion probe and method for preparing sample target of ion probe |
| CN112525976A (en) * | 2020-10-19 | 2021-03-19 | 中国科学院广州地球化学研究所 | Method for simultaneously analyzing water content, oxygen isotope and hydrogen isotope in water-containing mineral based on large-scale ion probe |
| CN114264846A (en) * | 2021-12-20 | 2022-04-01 | 中国科学院地质与地球物理研究所 | Preparation method of ion probe sample target at specified position of fine particles |
| CN117388020A (en) * | 2023-09-28 | 2024-01-12 | 中山大学 | Sample target composed of diamond and inner mineral inclusion and preparation method thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108375497A (en) * | 2018-01-23 | 2018-08-07 | 中国科学院地质与地球物理研究所 | A kind of preparation method of secondary ion probe sample target |
| CN111141811A (en) * | 2019-12-26 | 2020-05-12 | 中国科学院地质与地球物理研究所 | Target holder assembly of ion probe and method for preparing sample target of ion probe |
| CN112525976A (en) * | 2020-10-19 | 2021-03-19 | 中国科学院广州地球化学研究所 | Method for simultaneously analyzing water content, oxygen isotope and hydrogen isotope in water-containing mineral based on large-scale ion probe |
| CN112525976B (en) * | 2020-10-19 | 2022-04-22 | 中国科学院广州地球化学研究所 | Method for simultaneously analyzing water content, oxygen isotope and hydrogen isotope in water-containing mineral based on large-scale ion probe |
| CN114264846A (en) * | 2021-12-20 | 2022-04-01 | 中国科学院地质与地球物理研究所 | Preparation method of ion probe sample target at specified position of fine particles |
| CN114264846B (en) * | 2021-12-20 | 2024-03-12 | 中国科学院地质与地球物理研究所 | Preparation method of ionic probe sample target of fine particle designated layer |
| CN117388020A (en) * | 2023-09-28 | 2024-01-12 | 中山大学 | Sample target composed of diamond and inner mineral inclusion and preparation method thereof |
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| CN107449648B (en) | 2019-09-27 |
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