CN109239179A - The measuring method of trace impurity in a kind of high purity aluminium oxide polycrystal material - Google Patents
The measuring method of trace impurity in a kind of high purity aluminium oxide polycrystal material Download PDFInfo
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- CN109239179A CN109239179A CN201810981555.7A CN201810981555A CN109239179A CN 109239179 A CN109239179 A CN 109239179A CN 201810981555 A CN201810981555 A CN 201810981555A CN 109239179 A CN109239179 A CN 109239179A
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Abstract
The present invention is a kind of measuring method of trace impurity in high purity aluminium oxide polycrystal material.The measuring method of impurity element in a kind of high purity aluminium oxide polycrystal material, comprising: (1) blocky high purity aluminium oxide polycrystal material sample is broken into polycrystalline particle；(2) it takes polycrystalline particle to be placed between two pieces of high-purity tantalum pieces, pressurizes, inlay to the surface of high-purity tantalum piece；(3) high-purity tantalum piece is put into GD-MS sample clamp, the one side for being inlaid with high purity aluminium oxide polycrystal material is detection faces；(4) ion source vacuumizes, and adjusts discharge voltage and discharge current in the pulsing mode；(5) pulse glow discharge spectrometer analysis is carried out under conditions of step (4) are set, and is acquired the signal strength of element to be measured, is calculated the mass fraction of impurity element to be measured.The measuring method avoids due to the influence that aluminum oxide polycrystal sample is irregular or surface roughness is to electric discharge and testing result, can be directly used for the impurity determination of high-purity alpha-alumina polycrystal material.
Description
Technical field
Present invention relates particularly to a kind of measuring methods of trace impurity in high purity aluminium oxide polycrystal material.
Background technique
With the fast development of LED industry, demand of the industry to the sapphire substrate sheet of high quality is more and more.Sapphire
As a kind of high temperature resistant and erosion-resisting high purity aluminium oxide polycrystalline material, there is excellent optical property, mechanical performance and chemistry
Stability, intensity is high, hardness is big, resistance to erosion, can work under the mal-condition close to 2000 DEG C of high temperature, be modern industry and light
The particularly important basic material of electronic industry.But the purity of high purity aluminium oxide directly affects the microstructure and property of its product
Can, therefore it is particularly significant to the Detection & Controling of impurity element in high purity aluminium oxide.
Since high purity aluminium oxide is high-melting-point, high boiling insoluble compound, poorly conductive, purity is high, in sample making course
It easily pollutes, so that the quality testing enforcement difficulty of high purity aluminium oxide is larger.All the time, high purity aluminium oxide sample is accurate fixed
Amount detects at home or even is in the world always a biggish problem.Although China just has begun industrialization before more than ten years
High purity aluminium oxide is produced, but there are no the professional standard of high purity aluminium oxide impurity analysis and national standards so far.
Currently, the measuring method of the impurity for aluminium oxide, generally using x ray fluorescence spectrometry, extraction spectrophotometric method and
Inductively coupled plasma atomic emission spectrometry.
X ray fluorescence spectrometry, there are serious matrix effect, is unable to satisfy high purity aluminium oxide since it detects limit for height
The analysis requirement of sample, is not used to the impurity determination of high-purity alpha-alumina.
Fe in extraction spectrphotometric method for measuring high purity aluminium oxide2O3、SiO2Content, using inductively coupled plasma body atomic emissions
Impurity element in spectrographic determination high purity aluminium oxide.Due to extraction spectrophotometric method and inductively coupled plasma atomic emission spectrometry
It is to need sample being dissolved into liquid solution and detect using wet chemical sample preparation；And high purity aluminium oxide is high-melting-point, height
The insoluble compound of boiling point, is difficult under normal temperature and pressure to decompose and insoluble in bronsted lowry acids and bases bronsted lowry, and due to high purity aluminium oxide polycrystal material purity
Height, the pollution that chemical reagent etc. is highly prone in course of dissolution, influence testing result；In addition, this method sample preparation procedure
Complexity, disturbing factor are more, have significant limitation, are not used to the impurity determination of high-purity alpha-alumina.
Glow discharge spectrometry (GD-MS) as solid conductive material is directly carried out trace and ultratrace element analysis
Most effective means are widely used to the analysis of the materials such as various high pure metals, alloy in recent years.Wherein, U.S.'s match is silent flies
The Element-GD type glow discharge mass spectroscopy that your Science and Technology Ltd. of generation produces is most widely used in China.But it uses
It is had the following problems during GD-MS measurement impurity element, leads to not the impurity determination for being directly used in high-purity alpha-alumina:
(1) patent CN 201310302981.0 mixes in proportion alumina powder and copper powder, then by mixed powder
Last tabletting, using impurity element in direct current glow discharge mass spectrometric determination Alpha-alumina.Due to GD-MS in continuous mode by sample
Product are directly as the cathode of glow discharge, therefore it is required that sample has good electric conductivity, and sample itself property and surface are thick
Rough degree can generate a degree of influence to electric discharge and testing result.Alumina powder is mixed pressure with copper powder by this method
Therefore piece, sample have electric conductivity.But the method for making sample has biggish shortcomings and limitations: it is high-purity to be 1. only applicable to α type
The measurement of alumina powder samples is not suitable for the measurement of blocky high purity aluminium oxide polycrystal material；2. selecting high-purity copper powder as
Two cathode materials cannot achieve and detect to the critical impurities elemental copper in high purity aluminium oxide product as quality control, and
The elements such as major impurity element of Fe, Si, Na in high-purity copper powder are also the impurity element being primarily upon in high purity aluminium oxide product,
It is easy to produce bigger effect the accuracy of testing result；3. the more difficult assurance of mixing match, is easy to draw during sample blending
Into impurity, and the moisture of powder sample adsorption and air may cause sample avalanche in discharge process, to glow discharge
It generates larger interference and influences measurement result.
(2) non-conductive material is processed into bar samples by patent CN 201010606816.0；Indium metal is placed in quartzy earthenware
Molten condition is heated in crucible；Non-conductive sample surfaces carry out glow discharge mass spectrometry analysis after coating one layer of indium metal film.The party
Non-conductive sample surfaces are coated one layer of indium metal and carry out GD-MS measurement by method, since high purity indium fusing point is lower, need to it is lower from
Carried out at a temperature of component analysis, the sample preparation and test method be only suitable for VG9000 type GD-MS (stopped production in 2005, from
Component is cooling using liquid nitrogen), it is not suitable for the widely used Element type GD-MS in the current world (ion source, which is adopted, to be water-cooled)
Measurement, have biggish limitation；Furthermore sample preparation procedure is more complicated, using easily drawing in silica crucible melting process
Into impurity, the accuracy of testing result is influenced.
In view of this, the present invention proposes a kind of measuring method of trace impurity in high purity aluminium oxide polycrystal material, the party
Method can be to avoid since aluminum oxide polycrystal sample is irregular or influence of the surface roughness to electric discharge and testing result；Sample system
It for simple, quick, Determination Limit is low, discharges similar with conductor sample, is easy stabilization and signal stabilization is good, can be directly used for height
The impurity determination of Purity Alumina polycrystal material.
Summary of the invention
The purpose of the present invention is to provide a kind of measuring method of trace impurity in high purity aluminium oxide polycrystal material, by
High-purity tantalum piece is mixed and made into cathode conductor material as the second cathode, using High-purity Tantalum and high purity aluminium oxide polycrystal material, thus real
Existing glow discharge mass spectroscopy analyzes the measurement of the blocky non-conductive material such as high purity aluminium oxide polycrystal material, avoids due to aluminium oxide
The influence that Polycrystalline is irregular or surface roughness is to electric discharge and testing result；Sample preparation is simple, quickly, Determination Limit
It is low, it discharges similar with conductor sample, is easy stabilization and signal stabilization is good, precision with higher can be directly used for high-purity
Spend the impurity determination of alumina polycrystalline material.
To achieve the goals above, used technical solution are as follows:
The measuring method of impurity element in a kind of high purity aluminium oxide polycrystal material, comprising the following steps:
(1) blocky high purity aluminium oxide polycrystal material sample to be measured is crushed, is processed into polycrystalline particle；
(2) it takes a polycrystalline particle to be placed between two pieces of high-purity tantalum pieces, pressurizes, inlay polycrystalline particle to high-purity tantalum piece
Surface；
(3) the high-purity tantalum piece for inlaying polycrystalline particle is put into GD-MS sample clamp, is inlaid with high purity aluminium oxide polycrystal material
One side be detection faces, and the position for making to be inlaid with polycrystal material is located at the center in excitation hole；
(4) ion source vacuumizes, and adjusts discharge voltage and discharge current, discharge voltage 0.8- in the pulsing mode
1.2kV, burst length are 40-100 μ s, discharge gas flow 350-750mL/min；It is tuned by ion source by intermediate-resolution
Greater than 3800, high-resolution is greater than 8000；
(5) pulse glow discharge spectrometer analysis is carried out under conditions of step (4) are set, and acquires the signal of element to be measured
Intensity calculates the mass fraction of impurity element to be measured.
Further, in the step (1), the diameter of polycrystalline particle is 2-4mm.
Further, in the step (2), the purity of high-purity tantalum piece should be not less than 99.999%, and Na, Mg, Si, Ca,
The single impurity content of Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Ga should be not more than 0.05 μ g/g.
Further, in the step (2), high-purity tantalum piece with a thickness of 0.5-10mm；
Further, high-purity tantalum piece is round sheet or rectangular sheet.
Further, high-purity tantalum piece diameter of the round sheet is 20-30mm；
The High-purity Tantalum leaf length and width of the rectangular sheet are 20-30mm.
Further, in the step (2), high-purity tantalum piece needs to clean before use.
Further, the cleaning are as follows: the mixed solution of the nitric acid and hydrofluoric acid that are first 3:1 with volume ratio carries out corruption
Erosion, then after being cleaned with pure water, with washes of absolute alcohol, drying.
Further, in the step (4), in the pulsing mode, by sputtering, it is ensured that differentiate peak intensity in matrix Al27
Greater than 1 × 109Cps, the ratio between matrix Ta181 and the peak intensity of matrix Al27 should be less than 10, and the matrix peak to Al27 and Ta181 is steady
Pre-sputtering 15-30min after fixed.
Further, in the step (4), using Element GD type glow discharge mass spectroscopy, in the pulsing mode,
Discharge voltage 0.8kV is set, the burst length is 80 μ s, discharge gas flow 650mL/min；The matrix peak of Al27 and Ta181
Pre-sputtering 15min after stabilization.
Compared with prior art, the beneficial effects of the present invention are:
1, in a kind of high purity aluminium oxide polycrystal material of the present invention trace impurity measuring method, in High-purity Tantalum often
See that the impurity elements such as Nb, Mo, W there's almost no in high purity aluminium oxide product, largely avoids the second cathode material
Bring interference；By high-purity tantalum piece as the second cathode, cathode is mixed and made into using High-purity Tantalum and high purity aluminium oxide polycrystal material
Conductor material, thus realize that glow discharge mass spectroscopy analyzes the measurement of the blocky non-conductive material such as high purity aluminium oxide polycrystal material,
It avoids to discharge to GD-MS due to factors such as high purity aluminium oxide polycrystal material is in irregular shape, rough surface, out-of-flatnesses and detect and tie
The influence of fruit, GD-MS analysis can not directly be carried out by solving the problems, such as that high purity aluminium oxide polycrystal material is non-conductive.
2, in a kind of high purity aluminium oxide polycrystal material of the present invention trace impurity measuring method, using wide at present
The Element-GD type glow discharge mass spectroscopy of Thermo Fisher Scientific Inc. of U.S. production of general application, establishes one kind
Sample preparation procedure is simple, the method that can effectively avoid pollution；It discharges in the test method similar with conductor sample, is easy to stablize
And signal stabilization is good, signal-to-noise ratio (S/N) is ideal, and detection speed is fast, analysis precision is high.
3, in a kind of high purity aluminium oxide polycrystal material of the present invention trace impurity measuring method, with other detection
Method is compared, and this invention simplifies cumbersome sample pre-treatments step, meets rapid multi-element analysis in modern high-purity material
It is required that also having opened up thinking to impurity content in the other kinds of non-conductive sample of measurement.
4, in a kind of high purity aluminium oxide polycrystal material of the present invention trace impurity measuring method, provide one kind
It is simple to operation, and interfere less, precision it is good, be well positioned to meet multiple trace impurities in high purity aluminium oxide polycrystal material while detecting
Method, meet scientific research, production detection the needs of.
Specific embodiment
For the measuring method of trace impurity in a kind of the present invention is further explained high purity aluminium oxide polycrystal material, reach
It is expected that goal of the invention, in conjunction with the preferred embodiment, to trace in a kind of high purity aluminium oxide polycrystal material proposed according to the present invention
The measuring method of impurity element, specific embodiment, structure, feature and its effect, detailed description is as follows.In following the description
In, what different " embodiment " or " embodiment " referred to is not necessarily the same embodiment.In addition, the spy in one or more embodiments
Determining feature, structure or feature can be combined by any suitable form.
In elaborating a kind of high purity aluminium oxide polycrystal material of the present invention before the measuring method of trace impurity, having must
The method etc. referred in the present invention is described further, to reach better effect.
The working principle of glow discharge spectrometry (abbreviation GD-MS): by sample be installed to glow discharge mass spectroscopy it is equal from
Daughter arc chamber hits specimen surface using the ion that inert gas (high-purity argon gas) generates under high voltages, brings it about and splash
It penetrates, the atom that sample sputtering generates, which diffuses in plasma, to be ionized.Then, ion enters mass analyzer, due to not
There is different mass-to-charge ratioes with ion, mass analyzer separates different ions according to mass-to-charge ratio, finally by ion detector
It is detected and is counted.
The purity of high-purity tantalum piece employed in the present invention should be not less than 99.999%, and Na, Mg, Si, Ca, Ti, V, Cr,
The single impurity content of Mn, Fe, Ni, Cu, Zn, Ga should be not more than 0.05 μ g/g.It is with a thickness of 0.5-10mm；When for circular piece
Diameter is 20-30mm when shape；When being 20-30mm for rectangular sheet duration degree and width.
After having understood above method etc., below in conjunction with specific embodiment to a kind of high purity aluminium oxide polycrystalline of the present invention
The measuring method of trace impurity is further described in detail in material:
In the examples below: the content of the typical element detected with different time sections characterizes the electric discharge of the method for the present invention
Stability, the numerical value detected each time is closer, illustrates that discharge stability is better；The typical case's member detected with different time sections
The analysis repeatability of relative standard deviation (RSD%) characterization the method for the present invention of cellulose content, this numerical value is smaller, illustrates analysis weight
Renaturation is better.
Embodiment 1.
(1) bulk high purity aluminium oxide polycrystal material Sample A P1# to be measured is crushed, is processed into the particle that diameter is 2-4mm and tries
Sample；Bring in operating process is avoided to pollute in sample process.
(2) mixed solution of the nitric acid and hydrofluoric acid that are first 3:1 with volume ratio corrodes high-purity tantalum piece, then uses pure water
After cleaning, with washes of absolute alcohol, drying；
After taking the high purity aluminium oxide polycrystalline particle of a 2.5mm to be placed in two pieces of cleanings high-purity tantalum piece (thickness 0.5mm, it is pure
Degree >=99.999%, and the single impurity content of Na, Mg, Si, Ca, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Ga should be not more than
0.05μg/g；Length × wide=25mm × 25mm)；Under the pressure of 2KN or so, using SYP-30TS Manual tablet pressing machine, (Shanghai is new
Promise instrument), inlay polycrystalline particle to the surface of high-purity tantalum piece.
High-purity tantalum piece with good conductivity is introduced as the second cathode, high purity aluminium oxide polycrystalline material to be measured is inlayed to high-purity
The surface of tantalum piece keeps originally nonconducting sample conductive, carries out glow discharge mass spectroscopy measurement.
(3) in the GD-MS sample clamp for being put into high-purity tantalum piece, the one side of high purity aluminium oxide polycrystal material is inlaid with as detection
Face, and the position for being inlaid with polycrystal material is made to be located at the center for exciting hole；
(4) it selects aluminium for matrix, carries out pulse glow discharge spectrometer analysis.Specifically:
Using Element GD type glow discharge mass spectroscopy (Thermo Fisher Scientific Inc. of the U.S.), in pulse mode
Lower adjusting discharge voltage and discharge current set discharge voltage as 0.8kV, and the burst length is 80 μ s, and discharge gas flow is
650mL/min；Intermediate-resolution is greater than 3800 by ion source tuning, high-resolution is greater than 8000；It is sputtered after a period of time, really
It protects in matrix Al27 and differentiates peak intensity greater than 1 × 109Cps, the ratio between matrix Ta181 and the peak intensity of matrix Al27 should be less than 10,
The pre-sputtering 15min after the matrix peak of Al27 and Ta181 is stablized.
Pulse glow discharge spectrometer analysis is carried out under the above conditions, is acquired the signal strength of element to be measured, is calculated
The mass fraction of impurity element to be measured is measured in parallel 6 times, carries out data processing, obtains high purity aluminium oxide polycrystal material trace impurity member
The concentration of element, testing result are shown in Table 1.
1. high purity aluminium oxide polycrystal material Sample A P1# testing result of table
Laboratory comparative example is authoritative laboratory detection result, and detection method, instrument are had any different.
From 1 result of table: when being analyzed with the method for the present invention high purity aluminium oxide polycrystal material Sample A P1#, different time sections
The RSD% of the typical element content detected is respectively less than 15.8%, discharges similar with conductor sample, is easy stabilization and signal stabilization
Property it is good, there is analysis repeatability very well, and each element test result is consistent, and it is quick to can be used for detecting multielement in high purity aluminium oxide
Analysis.
The measuring method of trace impurity in a kind of high purity aluminium oxide polycrystal material described in the embodiment of the present invention, by height
Pure tantalum piece is mixed and made into cathode conductor material as the second cathode, using High-purity Tantalum and high purity aluminium oxide polycrystal material, to realize
Glow discharge mass spectroscopy analyzes the measurement of the blocky non-conductive material such as high purity aluminium oxide polycrystal material, avoids since aluminium oxide is more
The influence that brilliant sample is irregular or surface roughness is to electric discharge and testing result；Sample preparation is simple, quickly, Determination Limit
It is low, it discharges similar with conductor sample, is easy stabilization and signal stabilization is good, precision with higher can be directly used for high-purity
The impurity determination for spending aluminium oxide meets the needs of scientific research, production detection.
Embodiment 2.
Specific steps are as follows:
(1) blocky high purity aluminium oxide polycrystal material sample to be measured is crushed AP2#, is processed into the particle that diameter is 2-4mm and tries
Sample；Bring in operating process is avoided to pollute in sample process.
(2) mixed solution of the nitric acid and hydrofluoric acid that are first 3:1 with volume ratio corrodes high-purity tantalum piece, then uses pure water
After cleaning, with washes of absolute alcohol, drying；
Take the high purity aluminium oxide polycrystalline particle of a 3.5mm in two pieces cleaning after high-purity tantalum piece (thickness 8mm, purity >=
99.999%, and the single impurity content of Na, Mg, Si, Ca, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Ga should be not more than 0.05 μ
G/g, length × wide=25mm × 25mm)；Under the pressure of 2KN or so, using SYP-30TS Manual tablet pressing machine (the new promise instrument in Shanghai
Device), inlay polycrystalline particle to the surface of high-purity tantalum piece；
(3) in the GD-MS sample clamp for being put into high-purity tantalum piece, the one side of high purity aluminium oxide polycrystal material is inlaid with as detection
Face, and the position for being inlaid with polycrystal material is made to be located at the center for exciting hole；
(4) it selects aluminium for matrix, carries out pulse glow discharge spectrometer analysis.Specifically:
Using Element GD type glow discharge mass spectroscopy (Thermo Fisher Scientific Inc. of the U.S.), in pulse mode
Lower adjusting discharge voltage and discharge current set discharge voltage as 1.2kV, and the burst length is 100 μ s, and discharge gas flow is
350mL/min；Intermediate-resolution is greater than 3800 by ion source tuning, high-resolution is greater than 8000；It is sputtered after a period of time, really
It protects in matrix Al27 and differentiates peak intensity greater than 1 × 109Cps, the ratio between matrix Ta181 and the peak intensity of matrix Al27 should be less than 10,
The pre-sputtering 30min after the matrix peak of Al27 and Ta181 is stablized.
Pulse glow discharge spectrometer analysis is carried out under the above conditions, is acquired the signal strength of element to be measured, is calculated
The mass fraction of impurity element to be measured is measured in parallel 6 times, carries out data processing, obtains high purity aluminium oxide polycrystal material trace impurity member
The concentration of element, testing result are shown in Table 2.
2. high purity aluminium oxide polycrystal material Sample A P2# testing result of table
Laboratory comparative example is authoritative laboratory detection result, and detection method, instrument are had any different.
From 2 result of table table: when being analyzed with the method for the present invention high purity aluminium oxide polycrystal material Sample A P2#, different time
The RSD% for the typical element content that section detects is respectively less than 17.0%, discharges similar with conductor sample, is easy stabilization and signal is steady
It is qualitative good, there is analysis repeatability very well, and each element test result is consistent, and it is fast to can be used for detecting multielement in high purity aluminium oxide
Speed analysis.
The measuring method of trace impurity in a kind of high purity aluminium oxide polycrystal material described in the embodiment of the present invention, by height
Pure tantalum piece is mixed and made into cathode conductor material as the second cathode, using High-purity Tantalum and high purity aluminium oxide polycrystal material, to realize
Glow discharge mass spectroscopy analyzes the measurement of the blocky non-conductive material such as high purity aluminium oxide polycrystal material, avoids since aluminium oxide is more
The influence that brilliant sample is irregular or surface roughness is to electric discharge and testing result；Sample preparation is simple, quickly, Determination Limit
It is low, it discharges similar with conductor sample, is easy stabilization and signal stabilization is good, precision with higher can be directly used for high-purity
The impurity determination for spending aluminium oxide meets the needs of scientific research, production detection.
The above is only the preferred embodiment of the embodiment of the present invention, not makees any shape to the embodiment of the present invention
Limitation in formula, any simple modification to the above embodiments of technical spirit according to an embodiment of the present invention, equivalent variations
With modification, in the range of still falling within technical solution of the embodiment of the present invention.
Claims (10)
1. the measuring method of impurity element in a kind of high purity aluminium oxide polycrystal material, which comprises the following steps:
(1) blocky high purity aluminium oxide polycrystal material sample to be measured is crushed, is processed into polycrystalline particle；
(2) it takes a polycrystalline particle to be placed between two pieces of high-purity tantalum pieces, pressurizes, inlay polycrystalline particle to the table of high-purity tantalum piece
Face；
(3) the high-purity tantalum piece for inlaying polycrystalline particle is put into GD-MS sample clamp, is inlaid with the one of high purity aluminium oxide polycrystal material
Face is detection faces, and the position for being inlaid with polycrystal material is made to be located at the center for exciting hole；
(4) ion source vacuumizes, and adjusts discharge voltage and discharge current, discharge voltage 0.8-1.2kV, arteries and veins in the pulsing mode
Rushing the time is 40-100 μ s, discharge gas flow 350-750mL/min；It is tuned by ion source and is greater than intermediate-resolution
3800, high-resolution is greater than 8000；
(5) pulse glow discharge spectrometer analysis is carried out under conditions of step (4) are set, the signal for acquiring element to be measured is strong
Degree, calculates the mass fraction of impurity element to be measured.
2. measuring method according to claim 1, which is characterized in that wherein,
In the step (1), the diameter of polycrystalline particle is 2-4mm.
3. measuring method according to claim 1, which is characterized in that wherein,
In the step (2), the purity of high-purity tantalum piece should be not less than 99.999%, and Na, Mg, Si, Ca, Ti, V, Cr, Mn, Fe,
The single impurity content of Ni, Cu, Zn, Ga should be not more than 0.05 μ g/g.
4. measuring method according to claim 1, which is characterized in that wherein,
In the step (2), high-purity tantalum piece with a thickness of 0.5-10mm.
5. measuring method according to claim 4, which is characterized in that wherein,
High-purity tantalum piece is round sheet or rectangular sheet.
6. measuring method according to claim 5, which is characterized in that wherein,
High-purity tantalum piece diameter of the round sheet is 20-30mm；
The High-purity Tantalum leaf length and width of the rectangular sheet are 20-30mm.
7. measuring method according to claim 1, which is characterized in that wherein,
In the step (2), high-purity tantalum piece needs to clean before use.
8. measuring method according to claim 7, which is characterized in that wherein,
The cleaning are as follows: the mixed solution of the nitric acid and hydrofluoric acid that are first 3:1 with volume ratio is corroded, then is cleaned with pure water
Afterwards, with washes of absolute alcohol, drying.
9. measuring method according to claim 1, which is characterized in that wherein,
In the step (4), in the pulsing mode, by sputtering, it is ensured that differentiate peak intensity in matrix Al27 and be greater than 1 × 109Cps,
The ratio between the peak intensity of matrix Ta181 and matrix Al27 should be less than 10, the pre-sputtering 15- after the matrix peak of Al27 and Ta181 is stablized
30min。
10. measuring method according to claim 9, which is characterized in that wherein,
In the step (4), using Element GD type glow discharge mass spectroscopy, in the pulsing mode, discharge voltage is set
0.8kV, burst length are 80 μ s, discharge gas flow 650mL/min；Pre-sputtering after the matrix peak of Al27 and Ta181 is stablized
15min。
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| CN110470724A (en) * | 2019-09-19 | 2019-11-19 | 广东先导稀材股份有限公司 | The measuring method of trace impurity in a kind of high-purity silicon dioxide |
| 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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| CN114512764A (en) * | 2022-02-21 | 2022-05-17 | 上海凯矜新材料科技有限公司 | Nano alumina diaphragm paint and preparation method thereof |
| CN116337682A (en) * | 2023-05-23 | 2023-06-27 | 江苏沙钢集团有限公司 | Method for detecting molten steel yield of ball-milled particle steel hot-pressed block by adopting quartz crucible melting |
| CN116337682B (en) * | 2023-05-23 | 2023-08-18 | 江苏沙钢集团有限公司 | Method for detecting molten steel yield of ball-milled particle steel hot-pressed block by adopting quartz crucible melting |
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