CN107449648B - A kind of preparation method of the sample target of the ore mineral suitable for ion microprobe analysis - Google Patents
A kind of preparation method of the sample target of the ore mineral suitable for ion microprobe analysis Download PDFInfo
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- CN107449648B CN107449648B CN201710520161.7A CN201710520161A CN107449648B CN 107449648 B CN107449648 B CN 107449648B CN 201710520161 A CN201710520161 A CN 201710520161A CN 107449648 B CN107449648 B CN 107449648B
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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 methods of the sample target of ore mineral suitable for ion microprobe analysis, using alloy material instead of epoxy resin, target material hardness processed is moderate, it is suitble to grinding and buffing, it can effectively solve 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 fields, and in particular to it is a kind of suitable for ion microprobe analysis
The preparation method of the sample target of ore mineral.
Background technique:
Ore mineral individual particle is very small, such as zircon, and 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, basal diameter are 1 inch (25.4mm), and the optimum position of ion stream, is placed on sample for ore mineral when according to test
On position at product pinwheel 8-15mm.When carrying out sims analysis, sample target is put into the sample carrier of instrument, sample is utilized
Sample target is fixed in sample carrier by the baffle of the circular ring plate and the back side that hold in the palm edge 3mm wide.Conventional method is to glue list at present
Epoxy resin is poured in the mold of mineral, polishing is removed after completely cooling condensation, obtains a plane at ore mineral center,
Finally carry out dependence test.The target production technique is that have at low cost, and technique is simpler, and sample target high mechanical strength, shrinking percentage is low,
Performance is stablized, and has the advantages such as good cementitiousness, is most widely used at present sample target production method.But because of asphalt mixtures modified by epoxy resin
Rouge belongs to highly polar resin, has stronger compatibility to hydrone, has certain water absorption rate, be typical water-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 higher.Cause
, when sample target to be placed in vacuum environment, hydrone easily gets rid of the constraint of epoxy resin for this, is gradually released into sample cavity.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
Rouge " outgassing " is not enough to influence the analysis of the above element as a result, therefore not drawing attention to the destruction of vacuum.
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
When element analysis, when especially isotopic content relevant to H or O-H is analyzed (such as16O1H、1The elements such as H), or to vacuum
When spending more demanding elemental analysis, the molecules such as water 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 polish in advance mineral, and be pressed into indium according to certain orientation
In.And the Within Monominerals very tiny for granularity, it is difficult to the operation such as polished, polished in advance.
Very tiny for granularity is monomineralic16O1H、1In the analytic process of the elements such as H, epoxy resin " outgassing "
Extreme influence data validity, and when using pressure indium target, little particle Within Monominerals are difficult to be suppressed, before grinding and buffing etc.
Reason.Therefore one kind is urgently developed for the monomineralic target production technique of little particle, is convenient for pouring molding, sanding and polishing makes simple ore
Object exposes smooth test plane, without the sample target Target process of contaminated samples, influence sample cavity vacuum degree.
Summary of the invention:
The object of the present invention is to provide a kind of systems of the sample target of ore mineral suitable for ion microprobe analysis
Preparation Method, using alloy material instead of epoxy resin, while target material hardness processed is moderate, is suitble to sanding and polishing, can be effective
It solves 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 the ore mineral suitable for ion microprobe analysis, including following step
It is rapid:
1) ore mineral sample is fixed in the circle that glass core diameter is 8-15mm line by line, is 20- by diameter
The mold of 30mm is fixed to glass core, and mold is concentric with sample；
2) hardness is placed in vacuum drying oven heating melting in 50-250 DEG C of alloy material in 7-25HBW, fusing point, wait close
After golden material melts completely, the glass plate for being placed with sample and mold that step 1) is obtained is transferred in the same vacuum drying oven in advance
It is 5-10 minutes hot, molten alloy material is poured into mold, is vacuumized, is 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 continues constant temperature 0.5-1 hours, after being slowly cooled to room temperature in vacuum tank, takes out glass plate, removes mold, taking-up is poured
The sample target built carries out sanding and polishing to sample surfaces and sample target is made, and instrument can be packed into after cleaning and carries out sample test.
Before pouring, the glass plate for being placed with sample and mold is put in the vacuum drying oven of heating melting alloy material and is carried out
Preheating, in case rapid condensation-crystallization is precipitated alloy material to the cold.
Vacuum drying oven needs to deflate before carrying out slow cooling, temperature still need to be maintained at alloy material melting temperature it
On, after a certain period of time, slow cooling mode can be opened.
Preferably, the alloy material is Babbitt alloy material, tin-dominant, cadmium, bismuth, lead and other elements.
The ore mineral includes that zircon, olivine, apatite, quartz, pyrite, rutile, magnetic iron ore, cassiterite etc. are single
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, and effectively epoxy resin can be avoided in superelevation
In vacuum environment the problem of " outgassing ".
2) using alloy material of the invention and when being poured using the method for the present invention, mineral and the seamless rank of alloy material
It connects, made sample target hardness is moderate, can be carried out the operation such as polishing, polishing, and it is difficult effectively to solve pressure indium target small particles Within Monominerals
The problems such as with compacting, grinding and buffing.
In short, the present invention uses alloy material instead of epoxy resin, it can effectively avoid epoxy resin at high vacuum ring
In border the problem of " outgassing "；And target material hardness processed is moderate, is suitble to sanding and polishing；It can effectively solve indium target to little particle simple ore
Object is difficult to suppress, it is difficult to the problems such as carrying out sanding and polishing.
Detailed description of the invention:
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.
Specific embodiment:
It is to further explanation of the invention, rather than limiting the invention below.
Embodiment is using Wilson BH3000A type electricity Zi Bushi Durometer measurements formula to the hardness test of alloy material
The hardness of sample cross section, wherein hard alloy bulb diameter is 5mm, load 62.5kg, keeps 30s after indentation, 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, select zircon standard specimen: Qinghu, Penglai and Plesovices make as target sample processed, selection
The Babbitt alloy material 1 in table 1 is used as material, Fig. 1 is poured and illustrates the entire target surface after entire production.It can from Fig. 2
Out after sanding and polishing, available one very smooth zircon particle plane.
Specific steps are as follows:
The diameter that sticking double faced adhesive tape is drawn a circle to approve on a glass is to lay flat zircon standard specimen line by line viscous within the scope of the circle of 10mm
As on double-sided adhesive, and relative position is recorded.After the completion of sample placement, the PVC that internal diameter is 25mm is poured into mold
Glass core is sticked to, keeps mold concentric with sample, is gently compacted, makes to be seamlessly connected between mold and double-sided adhesive.Cut about 30g
Babbitt alloy material 1, is placed in Heating Cup, is put in heating melting in vacuum drying oven, after alloy material melts completely, will place
The glass plate of sample and mold is transferred in the same vacuum drying oven and preheats 5 minutes, and molten alloy material is poured into mold,
It opens vacuum pump to vacuumize, heating in vacuum, temperature is maintained on 10 DEG C of melting temperature of alloy material, constant temperature in vacuum environment
After 0.5 hour, vacuum pump is closed, opens vent valve, vacuum tank is made to be in normal pressure state, after continuing heated constant temperature 0.5 hour, is opened
Dynamic slow cooling program, when being slowly cooled to room temperature in vacuum tank, glass plate is taken out, and mold is removed from glass plate,
Take out the metal sample target poured.Whether observation sample target successfully pours, and otherwise needs to improve alloy material and melts, pours, very
The time that sky is stood and slow cooling is cooling.It, can examination with computer after finally the polishing of sample target, polishing and clean.Experiment knot
Fruit shows to be put into sample cavity when by resin target, it is found that vacuum degree reduces by 1 order of magnitude in sample cavity, over time,
Also it can not be evacuated to setting-out product initial vacuum level, and be put into the sample target of new method preparation, sample cavity vacuum degree has almost no change.
Embodiment 2:
In the present embodiment, select zircon standard specimen: Qinghu, Penglai, Plesovices, ZG1, ZG2, ZG3, ZG4 and
ZG5 is used as target sample processed, select to use in table 2 Babbitt alloy material 5 as material is poured, Fig. 3 is illustrated entirely make after
Entire target surface.As can be seen from Figure 4 after sanding and polishing, available one very smooth zircon particle plane.
Specific steps are as follows:
The diameter that sticking double faced adhesive tape is drawn a circle to approve on a glass is to lay flat zircon standard specimen line by line viscous within the scope of the circle of 10mm
It is recorded as on double-sided adhesive and to relative position.After the completion of sample placement, the PVC that internal diameter is 25mm is poured into mold and is glued
To glass core, keep mold concentric with sample, be gently compacted, makes to be seamlessly connected between mold and double-sided adhesive.Cut about 30g bars
Family name's alloy material 5, is placed in Heating Cup, is put in heating melting in vacuum drying oven, after alloy material melts completely, will place sample
The glass plate of product and mold is transferred in the same vacuum drying oven and preheats 5 minutes, and molten alloy material is poured into mold,
It opens vacuum pump to vacuumize, heating in vacuum, temperature is maintained on 10 DEG C of melting temperature of alloy material, constant temperature in vacuum environment
After 0.5 hour, vacuum pump is closed, opens vent valve, vacuum tank is made to be in normal pressure state, after continuing heated constant temperature 0.5 hour, is opened
Dynamic slow cooling program, when being slowly cooled to room temperature in vacuum tank, glass plate is taken out, and mold is removed from glass plate,
Take out the metal sample target poured.Observation sample target successfully pours.After the polishing of sample target, polishing and cleaning, it is placed in drying
It is stored in case.
Embodiment 3:
Reference implementation example 1, the difference is that Babbitt alloy material selects any in table 2 in Babbitt alloy material 2-4
Kind.
Claims (3)
1. a kind of preparation method of the sample target of the ore mineral suitable for ion microprobe analysis, which is characterized in that packet
Include following steps:
1) ore mineral sample is fixed in the circle that glass core diameter is 8-15mm line by line, is 20-30mm's by diameter
Mold is fixed to glass core, and mold is concentric with sample；
2) hardness is placed in vacuum drying oven heating melting in 50-250 DEG C of alloy material in 7-25HBW, fusing point, to alloy material
After material melting completely, the glass plate for being placed with sample and mold that step 1) is obtained, which is transferred in the same vacuum drying oven, preheats 5-
10 minutes, molten alloy material is poured into mold, is 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, opens vent valve, vacuum drying oven is in normal pressure, after
It is constant temperature 0.5-1 hours continuous, after being slowly cooled to room temperature in vacuum tank, glass plate is taken out, mold is removed, takes out the sample poured
Target carries out sanding and polishing to sample surfaces and sample target is made.
2. the preparation method of the sample target of the ore mineral according to claim 1 for ion microprobe analysis,
It is characterized in that, the ore mineral is Within Monominerals；Its main component of the alloy material be tin, cadmium, bismuth, two kinds in lead with
On.
3. the preparation method of the sample target of the ore mineral according to claim 2 for ion microprobe analysis,
It is characterized in that, the Within Monominerals include zircon, olivine, apatite, quartz, pyrite, rutile, magnetic iron ore, cassiterite.
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| CN107449648B true CN107449648B (en) | 2019-09-27 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108375497B (en) * | 2018-01-23 | 2020-03-24 | 中国科学院地质与地球物理研究所 | Preparation method of secondary ion probe sample target |
| CN111141811B (en) * | 2019-12-26 | 2020-10-16 | 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 |
| 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 |
| 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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