CN108918226A - A kind of preparation method of the titanium sponge detected for GDMS and titanium grain specimens - Google Patents
A kind of preparation method of the titanium sponge detected for GDMS and titanium grain specimens Download PDFInfo
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- 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
- G01N27/68—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 using electric discharge to ionise a gas
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Abstract
The present invention relates to a kind of titanium sponges and titanium grain specimens preparation method for GDMS detection, belong to analysis and testing technology field.It successively carries out ultrasonic cleaning, ultrapure water cleaning and organic reagent cleaning drying to high purity titanium crystal grain or little particle titanium sponge first；By high purity titanium crystal grain tabletting, formed to obtain high purity titanium crystalline substance tabletting if stacking dry plate；Pressurized, heated is carried out to the tabletting of high purity titanium crystalline substance or little particle titanium sponge, fusing is integrated, and obtains the tabletting of high purity titanium crystalline substance or titanium sponge sample；It places it in universal testing machine and is further pressed into required shape, ultrasonic cleaning is after finally polishing to get the titanium sponge or titanium grain specimens arrived for GDMS detection.
Description
Technical field
The present invention relates to a kind of titanium sponges and titanium grain specimens preparation method for GDMS detection, belong to analysis test skill
Art field.
Background technique
Titanium sponge is to be reacted by ilmenite with chlorine oxidation, becomes titanium tetrachloride, then be put into the stainless cylinder of steel of sealing, fills
With argon gas, biscuit titanium is made by magnesium metal reduction.Purity is generally 99.1-99.7%, and impurity content is
0.3%-0.9%, impurity element oxygen content are 0.06-0.20, and hardness (HB) is 100-157.Titanium sponge is production titanium, titanium valve
And the raw material of other titanium components.High purity titanium crystalline substance is titanium sponge resulting directly high-purity titanium products after the refining of electrorefining furnace,
Length 2-50mm, diameter 2-10mm, purity is up to 4N or more, and wherein oxygen content is lower than 200ppm.Titanium fusing point：1660 DEG C, boiling point：
3287 DEG C, density：4.54g/cm3.Titanium two big advantage the most outstanding is that specific strength height and corrosion resistance are strong, this just determines titanium
It is inevitable to have a extensive future in fields such as aerospace, weaponry, the energy, chemical industry, metallurgy, building, traffic, medicine.
There are many Determination of Impurity Elements method report in related pure titanium, current national standard method GB/T4698, HB7716-
2002 etc., it is chiefly used in content in the analysis of 0.005% or more single element, analytical cycle is long；When sample dissolution and processing, need
By sample preparation at bits sample, and need a large amount of strong acid and various redox and colour developing and complexing agent etc..
Glow discharge spectrometry (GDMS) is used as a kind of direct analytical technology of solid sample, is widely used to High Purity Gold
It is gone back in terms of the trace and ultratrace impurity of the materials such as category, semiconductor are analyzed, but it analyzes small size and irregular material sample
There are many difficulties, it is therefore desirable to which exploitation is suitble to the method for different sample detections to meet glow discharge mass spectrometry analysis method.
Chinese patent CN106198712A discloses trace impurity in a kind of glow discharge spectrometry detection metal and contains
The method of amount, although mentioning the patent in that patent can be used for the test of titanium, without being directed to titanium sponge and high purity titanium
Brilliant method for making sample.Industry standard methods include YS/T891-2013 high purity titanium chemical analysis method, i.e. trace impurity
Measurement and glow discharge spectrometry, but the sector standard method does not provide specifically for titanium sponge and high purity titanium crystalline substance sample yet
Preparation method.
Chinese patent 104458370A discloses a kind of preparation method of glow discharge mass spectroscopy analysis sample, which will
Metal powder sample, which is put into the graphite jig for be coated with release agent, makes powder compacting using the method for pressure sintering, surveys for GDMS
Examination, but the invention introduces release agent, is easy to fuse into powder sample in sintering, to introduce impurity element；And the invention
Only reach sample sintering without really combining together so that test when excitation signal it is discontinuous, test result repeatability and
Accuracy is relatively difficult to guarantee.Therefore, guarantee that sample is pollution-free and meets GDMS test sample specification in sample preparation procedure to want
It asks, the important leverage for being to provide analysis efficiency, guaranteeing analysis result preci-sion and accuracy.
Summary of the invention
The purpose of the present invention is overcoming above-mentioned shortcoming, a kind of titanium sponge and titanium crystal grain sample for GDMS detection is provided
The preparation method of product.
Technical solution of the present invention, a kind of preparation method of the titanium sponge detected for GDMS and titanium grain specimens are special
Sign is that steps are as follows：Ultrasonic cleaning is successively carried out to high purity titanium crystal grain or little particle titanium sponge first, ultrapure water cleans and has
The cleaning drying of machine reagent；By high purity titanium crystal grain tabletting, formed to obtain high purity titanium crystalline substance tabletting if stacking dry plate；To high purity titanium crystalline substance tabletting
Or little particle titanium sponge carries out pressurized, heated, fusing is integrated, and obtains the tabletting of high purity titanium crystalline substance or titanium sponge sample；Place it in ten thousand
Can testing machine be further pressed into required shape, finally polish after ultrasonic cleaning to get to for GDMS detection titanium sponge or
Titanium grain specimens.
The preparation method of the titanium sponge detected for GDMS and titanium grain specimens, steps are as follows：
(1) high purity titanium crystal grain or random little particle titanium sponge are placed in ultrasonic cleaning in cleaning solution, then with use
Ultrapure water cleaning, then dried up after being cleaned in organic reagent；
The high purity titanium crystal grain being surface-treated superposition is placed on the lower gasket of universal testing machine, if the sample that dry plate is superimposed
Product are pressed into sheet, obtain high purity titanium crystalline substance tabletting；
(2) step (1) the high purity titanium crystalline substance tabletting is placed in dedicated high purity graphite outer crucible or by little particle titanium sponge
It fills in high purity graphite outer crucible, compresses；Special graphite outer crucible is placed on the pallet of oxygen nitrogen instrument with crucible clamp and is carried out
Analysis；
(3) copper ring or copper pipe for taking ultrasonic cleaning clean are placed on the lower gasket of universal testing machine, by what is combined together
The tabletting of high purity titanium crystalline substance or titanium sponge sample are placed in copper ring or copper pipe center, and in surrounding gap, decimally titanium sponge filling is full；
The copper ring size that enabling universal testing machine controls entire tabletting carries out tabletting to it, the sample suppressed；
(4) coated abrasive working is carried out to the sample suppressed, then wipes dust with non-dust cloth, it is clear to be placed in ultrasonic wave in cleaning solution
It washes, is then cleaned with ultrapure water, then dried up after being cleaned in organic reagent spare.
2~8mm of high purity titanium crystal grain diameter, high 2~6mm described in step (1)；
Step (1) the ultrasonic cleaning time is 0.5-4min；
When suppressing in step (1) high purity titanium crystal grain, universal testing machine force value is controlled in 20~80KN.
When suppressing in step (1) high purity titanium crystal grain, the sample that 4~8 are superimposed is pressed into 8~15mm of diameter, high by 6~
The sheet of 12mm.
Degassing 200~500W of power is selected in step (2), analyzes 1600~7500W of power, 10~40s of degassing time, point
Analyse 20~200s of time；
Universal testing machine described in step (3), control compacting force value are pressed into core sample greatly in 20~100KN
It is small to be greater than Φ 8mm, while the copper ring size of entire tabletting is controlled, it is larger than the analysis aperture Φ of GDMS sample holder platform
19mm, and the thickness of entire tabletting is greater than 2mm.
Sand paper is specially the zirconium oxide sand paper that mesh number is 120 mesh in step (4)；
0.5~2min of ultrasonic cleaning is used in step (4).
The cleaning solution be cleaning solution be mass concentration be 6%~22% nitric acid, mass concentration be 3%~9% salt
Acid mixes in equal volume with the hydrofluoric acid that mass concentration is 3%~10%；
The organic reagent is dehydrated alcohol, one or more of arbitrary proportions are mixed in ether, acetone, carbon tetrachloride
It closes；Wherein ratio is volume ratio 30 when four kinds of mixing:1~10:1~10:1~10.
Graphite outer crucible is internal diameter Φ 13mm, outer diameter Φ 15mm, high 21mm in the step (1), and purity is greater than
99.999%；
The internal diameter of copper ring or copper pipe that step (3) is selected is greater than 20mm, 0.5~2.0mm of wall thickness, intercepts a height of 4~5mm.
Step (3) the oxygen nitrogen instrument when heating fusing sample, forbids logical oxygen under selected heating power.
The present invention breaches the limitation such as titanium sponge and small, the big, poor ductility of hardness of brilliant size of high purity titanium itself, has invented one
The new method for making sample of kind：It is first pressed into sheet, increases the contact area between piece and piece, then adjust high frequency on oxygen-nitrogen analyzer
The power of induction coil heats sample, them is made to combine together just, while guaranteeing not melting viscous wall, is convenient for from high purity graphite earthenware
It is poured in crucible, is subsequently placed in copper ring center, and by tabletting again after the filling of copper ring inner wall gap, be suitble to this
The size of GDMS analysis.
Beneficial effects of the present invention：The present invention is using multi-laminate adduction compacting high purity titanium crystalline substance and titanium sponge, then in high frequency
Sample is finally pressed into the size for meeting glow discharge spectrometry (GDMS) analysis by high-temperature fusion in induction furnace again.
The invention makes the original interlayer of sample and intergranular interface disappear, and is finally reached multiple high purity titanium crystalline substances and titanium sponge grain
It combines together, eliminates gap or the intralayer defects of sample interior, sample is avoided persistently to excite in glow discharge mass spectrometry (GDMS)
Data result is unstable in the process, to improve the precision of result.
Specific embodiment
Below in conjunction with embodiment, the present invention is further illustrated.
Embodiment 1
(1) diameter 6mm, high 6mm high purity titanium crystal grain are placed in nitric acid, mass concentration that mass concentration is 11% is 8%
Ultrasonic cleaning 0.5min in the cleaning solution that hydrochloric acid mixes in equal volume with the hydrofluoric acid that mass concentration is 6%, is cleaned with ultrapure water,
It is dried up after being cleaned in ether again.
(2) the high purity titanium crystal grain being surface-treated superposition is placed on the gasket of universal testing machine, force value controls 60KN, will
The sample of 5 superpositions is pressed into diameter 10mm, and high 6mm sheet guarantees to be put into completely in graphite outer crucible.
(3) high purity titanium crystalline substance tabletting is placed in dedicated high purity graphite outer crucible, with crucible clamp by special graphite outer crucible
It is placed on the pallet of oxygen nitrogen instrument, selects degassing power 300W, analyze power 3600W, degassing time 20s, analysis time 150s, prohibit
Only lead to oxygen, the high purity titanium crystalline substance wafer surface in high purity graphite outer crucible is made to melt and combine together.
(4) it is taken at the copper pipe that ultrasonic cleaning is clean in acetone, internal diameter 20mm, wall thickness 0.5mm intercept a height of 5mm, be placed in
On the lower gasket of universal testing machine, high purity titanium crystalline substance tabletting is placed in copper pipe center, decimally a titanium sponge is filled out in surrounding gap
It is full of.Universal testing machine is enabled, control compacting force value makes core sample be pressed into size greater than Φ 12mm, simultaneously in 80KN
The copper ring size for controlling entire tabletting is larger than the analysis aperture Φ 19mm of GDMS sample holder platform, and entire tabletting
Thickness be greater than 4mm.
(5) two surfaces for first using 120 mesh zirconium oxide coated abrasive workings to contact with sample in the sample suppressed, then use non-dust cloth
Dust is wiped, the hydrochloric acid that nitric acid, mass concentration that mass concentration is 11% are 8% and the hydrofluoric acid that mass concentration is 6% are placed in
Ultrasonic cleaning 1min, is cleaned with ultrapure water in the cleaning solution mixed in equal volume, then 3:1 ethyl alcohol：After-blow is cleaned in acetone
It does spare.
Embodiment 2
(1) random little particle titanium sponge is placed in the hydrochloric acid that nitric acid, mass concentration that mass concentration is 11% are 8%
Ultrasonic cleaning 1min is carried out in the cleaning solution mixed in equal volume with the hydrofluoric acid that mass concentration is 6%, is cleaned with ultrapure water, then
It is dried up after being cleaned in ether.
(2) little particle titanium sponge is placed in dedicated high purity graphite outer crucible, is compressed, it will be outside special graphite with crucible clamp
Crucible is placed on the pallet of oxygen nitrogen instrument, is selected degassing power 400W, is analyzed power 3200W, degassing time 10s, analysis time
120s forbids logical oxygen, makes the little particle titanium sponge surface melting in high purity graphite outer crucible and combine together.
(3) it is taken at the copper ring that ultrasonic cleaning is clean in acetone, internal diameter 20mm, wall thickness 1mm intercept a height of 4mm；It is placed in ten thousand
On the lower gasket of energy testing machine, titanium sponge tabletting is placed in copper ring center, decimally titanium sponge filling is full in surrounding gap.
Universal testing machine is enabled, control compacting force value makes core sample be pressed into size Φ 10mm in 60KN, while controlling entire pressure
The copper ring size that piece is crossed is larger than the analysis aperture Φ 19mm of GDMS sample holder platform, and the thickness of entire tabletting is greater than
2mm。
(4) two surfaces for first using 120 mesh zirconium oxide coated abrasive workings to contact with sample in the sample suppressed, then use non-dust cloth
Dust is wiped, the hydrochloric acid that nitric acid, mass concentration that mass concentration is 11% are 8% and the hydrofluoric acid that mass concentration is 6% are placed in
Ultrasonic cleaning 1min, is cleaned with ultrapure water in the cleaning solution mixed in equal volume, then is pressing 3:1:1:1 mixed dehydrated alcohol,
Ether, acetone, dried up after cleaning in carbon tetrachloride it is spare.
Preci-sion and accuracy test：Sample prepared by Examples 1 and 2 is put into GDMS sample stage, and carries out 15min
Pre-sputtering, investigate C, Si, Mn, Fe, Mg essential element, start when basicly stable with concentration acquire data, acquire 11 groups of data,
Its relative standard deviation (RSD%) is calculated, and is compared with the measurement result using ICP-MS and infrared C-S analyzer, is come with this
The repeatability and repeatability of evaluation analysis result, the results are shown in Table 1.
1 accuracy test result of table
This method verifies sample preparation with GDMS test result, and data result shows do not have using graphite crucible in table 1
Carbon content in sample is polluted, and the measurement relative deviation of essential element is smaller, and uses the mass spectrographic measured value of aura and inductance coupling
It is consistent to close plasma mass test result, is conducive to promote and apply.
A specific embodiment of the invention above described embodiment only expresses, but can not be therefore understands that for the present invention
The limitation of the scope of the patents.Any variation that those skilled in the art is the present invention under the enlightenment of present inventive concept is fallen
Within the scope of the present invention.
Claims (10)
1. a kind of preparation method of the titanium sponge detected for GDMS and titanium grain specimens, it is characterized in that steps are as follows：It is right first
High purity titanium crystal grain or little particle titanium sponge successively carry out ultrasonic cleaning, ultrapure water cleaning and organic reagent cleaning drying；It will be high
Pure titanium crystal grain tabletting forms to obtain high purity titanium crystalline substance tabletting if stacking dry plate；The tabletting of high purity titanium crystalline substance or little particle titanium sponge are carried out
Pressurized, heated, fusing are integrated, and obtain the tabletting of high purity titanium crystalline substance or titanium sponge sample；Universal testing machine is placed it in further to suppress
At required shape, ultrasonic cleaning is after finally polishing to get the titanium sponge or titanium grain specimens arrived for GDMS detection.
2. as described in claim 1 for the titanium sponge of GDMS detection and the preparation method of titanium grain specimens, it is characterized in that step
It is as follows：
（1）High purity titanium crystal grain or random little particle titanium sponge are placed in ultrasonic cleaning in cleaning solution, then used with ultrapure
Water cleaning, then dried up after being cleaned in organic reagent；
The high purity titanium crystal grain being surface-treated superposition is placed on the lower gasket of universal testing machine, if the sample pressure that dry plate is superimposed
Slabbing obtains high purity titanium crystalline substance tabletting；
（2）By step（1）The high purity titanium crystalline substance tabletting is placed in dedicated high purity graphite outer crucible or fills little particle titanium sponge
In in high purity graphite outer crucible, compress；Special graphite outer crucible is placed on the pallet of oxygen nitrogen instrument with crucible clamp and is analyzed；
（3）Copper ring that ultrasonic cleaning is clean or copper pipe is taken to be placed on the lower gasket of universal testing machine, it is high-purity by what is combined together
The tabletting of titanium crystalline substance or titanium sponge sample are placed in copper ring or copper pipe center, and in surrounding gap, decimally titanium sponge filling is full；It enables
The copper ring size that universal testing machine controls entire tabletting carries out tabletting to it, the sample suppressed；
（4）Coated abrasive working is carried out to the sample suppressed, then wipes dust with non-dust cloth, is placed in ultrasonic cleaning in cleaning solution,
It is then cleaned, then is dried up after being cleaned in organic reagent spare with ultrapure water.
3. as claimed in claim 2 for the titanium sponge of GDMS detection and the preparation method of titanium grain specimens, it is characterized in that：Step
（1）Described in 2 ~ 8mm of high purity titanium crystal grain diameter, high 2 ~ 6mm；
Step（1）The ultrasonic cleaning time is 0.5-4min；
Step（1）In to high purity titanium crystal grain suppress when, universal testing machine force value control in 20 ~ 80KN.
4. as claimed in claim 3 for the titanium sponge of GDMS detection and the preparation method of titanium grain specimens, it is characterized in that：Step
（1）In to high purity titanium crystal grain suppress when, by 4 ~ 8 be superimposed sample be pressed into 8 ~ 15mm of diameter, the sheet of high 6 ~ 12mm.
5. as claimed in claim 2 for the titanium sponge of GDMS detection and the preparation method of titanium grain specimens, it is characterized in that：Step
（2）Middle selection degassing 200 ~ 500W of power, analyzes 1600 ~ 7500W of power, 10 ~ 40s of degassing time, 20 ~ 200s of analysis time.
6. as claimed in claim 2 for the titanium sponge of GDMS detection and the preparation method of titanium grain specimens, it is characterized in that：Step
（3）Described in universal testing machine, control compacting force value makes core sample be pressed into size greater than Φ 8mm, together in 20 ~ 100KN
When control the copper ring size of entire tabletting, be larger than the analysis aperture Φ 19mm of GDMS sample holder platform, and entire pressure
The thickness of piece is greater than 2mm.
7. as claimed in claim 2 for the titanium sponge of GDMS detection and the preparation method of titanium grain specimens, it is characterized in that：Step
（4）Middle sand paper is specially the zirconium oxide sand paper that mesh number is 120 mesh；
Step（4）It is middle to use 0.5 ~ 2min of ultrasonic cleaning.
8. as claimed in claim 2 for the titanium sponge of GDMS detection and the preparation method of titanium grain specimens, it is characterized in that：It is described
Cleaning solution be cleaning solution be nitric acid, the hydrochloric acid that mass concentration is 3% ~ 9% and the mass concentration that mass concentration is 6% ~ 22% be 3% ~
10% hydrofluoric acid mixes in equal volume；
The organic reagent is dehydrated alcohol, one or more of arbitrary proportions are mixed in ether, acetone, carbon tetrachloride；Its
In four kinds of mixing when ratio be volume ratio 30:1~10:1~10:1~10.
9. as claimed in claim 2 for the titanium sponge of GDMS detection and the preparation method of titanium grain specimens, it is characterized in that：It is described
Step（1）Middle graphite outer crucible is internal diameter Φ 13mm, and outer diameter Φ 15mm, high 21mm, purity is greater than 99.999%；
Step（3）The copper ring of selection or the internal diameter of copper pipe are greater than 20mm, 0.5 ~ 2.0mm of wall thickness, intercept a height of 4 ~ 5mm.
10. as claimed in claim 2 for the titanium sponge of GDMS detection and the preparation method of titanium grain specimens, it is characterized in that：Institute
State step（3）Oxygen nitrogen instrument when heating fusing sample, forbids logical oxygen under selected heating power.
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| CN110865168A (en) * | 2019-11-15 | 2020-03-06 | 江苏隆达超合金航材有限公司 | Method for rapidly analyzing main amount, trace amount and trace elements in alloy slag |
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| CN110864949A (en) * | 2019-11-15 | 2020-03-06 | 江苏隆达超合金航材有限公司 | Preparation method of tungsten block sample for glow discharge mass spectrometry detection |
| CN112362595A (en) * | 2020-12-02 | 2021-02-12 | 成都光明派特贵金属有限公司 | Method for testing content of impurity elements in sponge platinum |
| CN113092228A (en) * | 2021-03-23 | 2021-07-09 | 宁波创润新材料有限公司 | Titanium crystal sample for GDMS detection and preparation method thereof |
| CN113109121A (en) * | 2021-04-22 | 2021-07-13 | 宁波江丰电子材料股份有限公司 | Sample preparation method and test method of trititanium pentoxide crystal particles in glow discharge mass spectrum |
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