CN113702485A - Method for measuring content of trace impurity elements in massive aluminum nitride - Google Patents
Method for measuring content of trace impurity elements in massive aluminum nitride Download PDFInfo
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- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title claims abstract description 52
- 238000000034 method Methods 0.000 title claims abstract description 45
- 239000012535 impurity Substances 0.000 title claims abstract description 20
- 229910052715 tantalum Inorganic materials 0.000 claims abstract description 33
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000002904 solvent Substances 0.000 claims abstract description 31
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 28
- 230000002378 acidificating effect Effects 0.000 claims abstract description 26
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 14
- 230000007797 corrosion Effects 0.000 claims abstract description 13
- 238000005260 corrosion Methods 0.000 claims abstract description 13
- 239000011259 mixed solution Substances 0.000 claims abstract description 10
- 238000005406 washing Methods 0.000 claims description 12
- 238000004544 sputter deposition Methods 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 5
- 239000008188 pellet Substances 0.000 claims description 5
- 238000001514 detection method Methods 0.000 abstract description 7
- 238000004458 analytical method Methods 0.000 abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 8
- 238000004140 cleaning Methods 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 238000012545 processing Methods 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 230000029087 digestion Effects 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000011895 specific detection Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000004891 communication Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000000705 flame atomic absorption spectrometry Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000001637 plasma atomic emission spectroscopy Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
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- 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
- G01N27/64—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 wave or particle radiation to ionise a gas, e.g. in an ionisation chamber
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Abstract
本发明涉及分析检测技术领域，公开了一种测定块状氮化铝中痕量杂质元素含量的方法。该方法包括：（1）将钽片与第一酸性溶剂进行第一接触，得到腐蚀钽片；以及将待测块状氮化铝样品与第二酸性溶剂进行第二接触，得到腐蚀待测块状氮化铝样品；其中，所述钽片上每间隔1‑2mm设有直径为1‑2mm的通孔；所述第一酸性溶剂、所述第二酸性溶剂均为用量体积比为5‑10:1的硝酸和氢氟酸混合溶液；将所述腐蚀钽片放置于所述腐蚀待测块状氮化铝样品上，并采用直流辉光放电质谱仪进行分析。本发明提供的方法操作简单，不容易引入污染，能够提高检测结果准确性。
The invention relates to the technical field of analysis and detection, and discloses a method for determining the content of trace impurity elements in bulk aluminum nitride. The method includes: (1) firstly contacting a tantalum sheet with a first acidic solvent to obtain a corroded tantalum sheet; and secondly contacting a bulk aluminum nitride sample to be tested with a second acidic solvent to obtain a corroded block to be tested aluminum nitride sample; wherein, the tantalum sheet is provided with a through hole with a diameter of 1-2mm at every interval of 1-2mm; the first acidic solvent and the second acidic solvent are both in a volume ratio of 5-10 : 1 mixed solution of nitric acid and hydrofluoric acid; the corrosion tantalum sheet is placed on the corrosion block aluminum nitride sample to be tested, and is analyzed by a DC glow discharge mass spectrometer. The method provided by the invention has simple operation, is not easy to introduce pollution, and can improve the accuracy of the detection result.
Description
Technical Field
The invention relates to the technical field of analysis and detection, in particular to a method for measuring the content of trace impurity elements in massive aluminum nitride.
Background
The aluminum nitride as the third-generation semiconductor material has the characteristics of good heat-conducting property, high volume resistivity, and small dielectric constant and dielectric loss, so that the aluminum nitride has wide application prospects in the aspects of super-large-scale dust collection circuit substrates, packaging, high-power communication equipment and the like.
However, the purity of aluminum nitride, such as the content of some metal elements (Mg, Fe, Si, etc.), directly affects the performance of aluminum nitride, and therefore, how to effectively detect impurities of aluminum nitride becomes important.
At present, the main methods for measuring the aluminum nitride impurities include flame atomic absorption spectrometry and plasma emission spectrometry. The two methods both need to digest the sample, and the aluminum nitride has good high temperature resistance and corrosion resistance, so that the digestion process is complex, other impurity pollution is easily introduced, and the accuracy of the detection result is reduced.
The glow discharge mass spectrometer can directly analyze a solid sample, avoids the digestion process of the sample, has higher sensitivity and extremely wide linear dynamic range, can measure the impurity elements with the content from ultra-trace to main body at one time, and has been widely applied to ultra-pure solid materials.
CN109239179A discloses a method for measuring impurity elements in high-purity alumina polycrystal, which is to press alumina polycrystal particles on a tantalum sheet and measure the impurity elements by adopting a pulse glow discharge mass spectrometer. However, aluminum nitride has high hardness and is difficult to adhere to tantalum sheets, and the method is not suitable for measuring non-conductive aluminum nitride.
Therefore, the method which is simple to operate and high in accuracy is developed to obtain the content of the trace impurity elements in the aluminum nitride, and the method has important significance.
Disclosure of Invention
The invention aims to overcome the defects that the method for measuring the content of trace impurity elements in aluminum nitride in the prior art is complex in operation, easy to introduce pollution and reduces the accuracy of a detection result.
In order to achieve the above object, the present invention provides a method for determining the content of trace impurity elements in bulk aluminum nitride, the method comprising:
(1) carrying out first contact on a tantalum sheet and a first acidic solvent to obtain a corrosion tantalum sheet; and
carrying out second contact on the blocky aluminum nitride sample to be detected and a second acidic solvent to obtain a blocky aluminum nitride sample to be detected through corrosion;
wherein, through holes with the diameter of 1-2mm are arranged on the tantalum sheet at intervals of 1-2 mm;
the first acidic solvent and the second acidic solvent are mixed solution of nitric acid and hydrofluoric acid with the dosage volume ratio of 5-10: 1;
(3) placing the corrosion tantalum sheet on the blocky aluminum nitride sample to be tested, and analyzing by using a direct current glow discharge mass spectrometer;
wherein the conditions of the direct current glow discharge mass spectrometer at least comprise: the discharge current is 1.5-2mA, the discharge voltage is 1000-1100V, and the pre-sputtering time is 5-10 min.
The method provided by the invention is simple to operate, pollution is not easy to introduce, and a matrix signal with strong and good stability can be obtained, so that the accuracy of a detection result is improved.
Drawings
FIG. 1 is a schematic view of via processing on a tantalum wafer according to example 1;
FIG. 2 is a schematic view showing the via hole processing in the tantalum sheet of example 2;
FIG. 3 is a schematic view of via processing on a tantalum wafer in comparative example 1;
FIG. 4 is a schematic view of via processing on a tantalum wafer in comparative example 2;
FIG. 5 shows the current values of Al at different times in examples 1 and 2.
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
In the present invention, unless otherwise specified, the room temperature or the room temperature means 25. + -. 2 ℃.
As previously mentioned, a first aspect of the present invention provides a method for determining the content of trace impurity elements in bulk aluminum nitride, the method comprising:
(1) carrying out first contact on a tantalum sheet and a first acidic solvent to obtain a corrosion tantalum sheet; and
carrying out second contact on the blocky aluminum nitride sample to be detected and a second acidic solvent to obtain a blocky aluminum nitride sample to be detected through corrosion;
wherein, through holes with the diameter of 1-2mm are arranged on the tantalum sheet at intervals of 1-2 mm;
the first acidic solvent and the second acidic solvent are mixed solution of nitric acid and hydrofluoric acid with the dosage volume ratio of 5-10: 1;
(4) placing the corrosion tantalum sheet on the blocky aluminum nitride sample to be tested, and analyzing by using a direct current glow discharge mass spectrometer;
wherein the conditions of the direct current glow discharge mass spectrometer at least comprise: the discharge current is 1.5-2mA, the discharge voltage is 1000-1100V, and the pre-sputtering time is 5-10 min.
It should be noted that the present invention has no special requirement on the kind of the dc glow discharge mass spectrometer, and only needs to be able to analyze and obtain the content of the trace impurity element in the bulk aluminum nitride, and the dc glow discharge mass spectrometer of the present invention is, for example, an Astrum type dc glow discharge mass spectrometer purchased from Nu Instruments.
In step (2), the etching tantalum sheet is placed on the bulk aluminum nitride sample to be etched and mounted together on the sheet holder support, so that the bulk aluminum nitride sample to be etched is exposed in the sputtering region.
Preferably, in step (1), the diameter of the through hole is 1mm or 2 mm. The inventors have found that with this preferred embodiment, a more stable and stronger matrix signal can be obtained.
Preferably, in the step (1), the first acidic solvent and the second acidic solvent are mixed solutions of nitric acid and hydrofluoric acid, and the volume ratio of the nitric acid to the hydrofluoric acid is 8-10: 1.
The concentration of the nitric acid and the concentration of the hydrofluoric acid are not particularly required in the present invention, and for example, the concentration of the nitric acid is 70 to 75wt% and the concentration of the hydrofluoric acid is 45 to 50wt% in the present invention.
Preferably, in step (1), the conditions of the first contacting include at least: the temperature is 20-40 deg.C, and the time is 2-5 min.
Preferably, in step (1), the conditions of the second contacting include at least: the temperature is 20-40 deg.C, and the time is 10-20 min.
Preferably, in the step (1), the tantalum pellet has a size of (12-40) × (12-40) × (0.1-0.3) mm, and the purity of the tantalum pellet is not less than 99.99 wt%.
Preferably, in the step (1), the size of the block-shaped aluminum nitride sample to be tested is (12-40) × (12-40) × (1-20) mm.
Preferably, in step (1), the method further comprises: and carrying out first washing and first drying on the material obtained by the first contact.
Preferably, in step (1), the method further comprises: and carrying out second washing and second drying on the material obtained by the second contact.
In the present invention, the solvent used for the first cleaning and the second cleaning, the amount of the solvent used and the number of times of the solvent used are not particularly required, and only the solvent used for rinsing the residual first acidic solvent or second acidic solvent is required, and for example, the solvent used for the first cleaning and the second cleaning is water, and the number of times of the first cleaning and the second cleaning is independently selected from 3 to 4 times.
The operation methods of the first drying and the second drying are not particularly required, and the cleaned flat sheet or the aluminum nitride sample is dried.
Preferably, in step (2), the conditions of the dc glow discharge mass spectrometer include at least: the discharge current is 1.5-1.8mA, the discharge voltage is 1000-1050V, and the pre-sputtering time is 8-10 min.
The present invention will be described in detail below by way of examples. In the following examples, various raw materials used are commercially available ones unless otherwise specified.
The bulk aluminum nitride sample to be tested: purchased from Nu Instruments;
flat sheet: purchased from conscientious color companies;
d.c. glow discharge mass spectrometer: type Astrum, available from Nu Instruments;
in the following examples, the analysis conditions of the dc glow discharge mass spectrometer were: the discharge current is 1.5mA, the discharge voltage is 1050V, and the pre-sputtering time is 10 min;
in the following examples, the concentrations of the nitric acid, the hydrofluoric acid and the ethanol were 71wt%, 49wt% and 99.7wt%, respectively;
in the following examples, the relative standard deviation is calculated as: (standard deviation/average content) × 100%.
Example 1
The embodiment provides a method for determining the content of trace impurity elements in bulk aluminum nitride, which comprises the following steps:
(1) corroding the processed tantalum sheet (the size is 15 multiplied by 0.2mm, through holes with the diameter of 1mm are formed at intervals of 1mm, see figure 1) with a first acidic solvent (a mixed solution of nitric acid and hydrofluoric acid with the dosage volume ratio of 10: 1) for 2min at room temperature, then washing with pure water for 3 times, washing with ethanol for 1 time, and airing to obtain a corrosion flat sheet; and
corroding a to-be-detected block aluminum nitride sample with the size of 20 multiplied by 1mm with a second acidic solvent (a mixed solution of nitric acid and hydrofluoric acid with the dosage volume ratio of 10: 1) for 10min at room temperature, then washing with pure water for 3 times, then washing with ethanol for 1 time, and then airing to obtain a to-be-detected block aluminum nitride sample;
(2) the thin tantalum sheet is covered on a blocky aluminum nitride sample and is arranged on a sheet holder support together, the aluminum nitride is ensured to be exposed in a sputtering area, the sample is pushed into a sample pool, a direct current glow discharge mass spectrometer is used for analysis, and specific detection results are shown in table 1.
Example 2
The embodiment provides a method for determining the content of trace impurity elements in bulk aluminum nitride, which comprises the following steps:
(1) corroding the processed tantalum sheet (the size is 15 multiplied by 0.2mm, through holes with the diameter of 2mm are formed at intervals of 1mm, see figure 2) with a first acidic solvent (a mixed solution of nitric acid and hydrofluoric acid with the dosage volume ratio of 10: 1) for 3min at room temperature, then washing with pure water for 4 times, washing with ethanol for 1 time, and airing to obtain a corroded tantalum sheet; and
corroding aluminum nitride with the size of 20 multiplied by 1mm with a second acidic solvent (a mixed solution of nitric acid and hydrofluoric acid with the dosage volume ratio of 10: 1) for 20min at room temperature, then washing with pure water for 4 times, then washing with ethanol for 1 time, and then airing to obtain a high-purity aluminum nitride sample to be corroded;
(2) the thin tantalum sheet is covered on a blocky aluminum nitride sample and is arranged on a sheet holder support together, the aluminum nitride is ensured to be exposed in a sputtering area, the sample is pushed into a sample pool, a direct current glow discharge mass spectrometer is used for analysis, and specific detection results are shown in table 2.
Comparative example 1
This comparative example measured the content of trace impurity elements in bulk aluminum nitride by the method of example 1, except that in step (1), 1 through-hole having a diameter of 3mm was opened in the tantalum pellet (see FIG. 3).
The rest of the procedure was the same as in example 1. The inventors found that the process signal of this comparative example was too low to detect.
Comparative example 2
This comparative example measured the content of trace impurity elements in bulk aluminum nitride by the method of example 3, except that in step (1), 1 through-hole having a diameter of 5mm was opened in the tantalum pellet (see FIG. 4).
The rest of the procedure was the same as in example 1. The inventors found that the process signal of this comparative example was too low to detect.
Table 1: test results of the aluminum nitride sample in example 1
Table 2: test results of the aluminum nitride sample in example 1
As can be seen from tables 1 and 2, when the method provided by the invention is used for detecting the content of the trace elements in the aluminum nitride, the surface pollution of the sample is small, the relative standard deviation of the detection is within 10%, and the precision is good.
The present invention exemplarily provides current values of Al at different times in example 1 and example 2, see fig. 5.
As can be seen from FIG. 5, the current value of Al can reach 5E-11 and the signal is stable when measured by the method provided by the present invention.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (10)
1. A method for determining the content of trace impurity elements in bulk aluminum nitride is characterized by comprising the following steps:
(1) carrying out first contact on a tantalum sheet and a first acidic solvent to obtain a corrosion tantalum sheet; and
carrying out second contact on the blocky aluminum nitride sample to be detected and a second acidic solvent to obtain a blocky aluminum nitride sample to be detected through corrosion;
wherein, through holes with the diameter of 1-2mm are arranged on the tantalum sheet at intervals of 1-2 mm;
the first acidic solvent and the second acidic solvent are mixed solution of nitric acid and hydrofluoric acid with the dosage volume ratio of 5-10: 1;
(2) placing the corrosion tantalum sheet on the blocky aluminum nitride sample to be tested, and analyzing by using a direct current glow discharge mass spectrometer;
wherein the conditions of the direct current glow discharge mass spectrometer at least comprise: the discharge current is 1.5-2mA, the discharge voltage is 1000-1100V, and the pre-sputtering time is 5-10 min.
2. The method of claim 1, wherein, in step (1), the through-hole has a straight diameter of 1mm or 2 mm.
3. The method according to claim 1 or 2, wherein in the step (1), the first acidic solvent and the second acidic solvent are mixed solutions of nitric acid and hydrofluoric acid in a volume ratio of 8-10: 1.
4. The method according to any one of claims 1 to 3, wherein in step (1), the conditions of the first contacting comprise at least: the temperature is 20-40 deg.C, and the time is 2-5 min.
5. The method according to any one of claims 1 to 4, wherein in step (1), the conditions of the second contacting comprise at least: the temperature is 20-40 deg.C, and the time is 10-20 min.
6. The method of any one of claims 1 to 5, wherein in step (1), the tantalum pellet has a size of (12-40) x (0.1-0.3) mm and a purity of not less than 99.99 wt%.
7. The method according to any one of claims 1 to 6, wherein in step (1), the size of the bulk aluminum nitride sample to be tested is (12-40) x (1-20) mm.
8. The method according to any one of claims 1-7, wherein in step (1), the method further comprises: and carrying out first washing and first drying on the material obtained by the first contact.
9. The method according to any one of claims 1-8, wherein in step (1), the method further comprises: and carrying out second washing and second drying on the material obtained by the second contact.
10. The method of any one of claims 1-9, wherein in step (2), the conditions of the dc glow discharge mass spectrometer comprise at least: the discharge current is 1.5-1.8mA, the discharge voltage is 1000-1050V, and the pre-sputtering time is 8-10 min.
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