CN115144459A - Method for detecting trace metal on surface of silicon carbide epitaxial wafer - Google Patents
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Abstract
The invention discloses a method for detecting trace metals on the surface of a silicon carbide epitaxial wafer, which comprises the following steps: adjusting the inductively coupled plasma mass spectrometer by using tuning liquid to tune the working conditions of the instrument; diluting the diluted standard sample solution into mixed standard solutions with different concentrations by using a clean volumetric flask and an analytical balance; the concentration gradient of each element is 0.00 mu g/L,0.10 mu g/L,0.20 mu g/L,0.50 mu g/L,1.00 mu g/L and 2.00 mu g/L; drawing a standard curve; sucking the back of the silicon carbide wafer by using a nonmetal vacuum suction pen, flatly placing the wafer, uniformly dripping 5ml of extracting solution on the center of the surface of the wafer by using a liquid transfer gun, slightly shaking the wrist to enable the solution to comprehensively and uniformly cover the whole surface of the wafer, staying for a moment, collecting the scanning solution into a PFA sample bottle, and performing on-machine test; the method can rapidly and accurately perform quantitative analysis on various metal elements on the surface of the silicon carbide epitaxial wafer, and ensure the controllable quality of the silicon carbide wafer.
Description
Technical Field
The invention belongs to the technical field of chemical detection methods, and particularly relates to a method for detecting trace metals on the surface of a silicon carbide epitaxial wafer by adopting a plasma mass spectrometry.
Background
At present, silicon carbide is an important basic material for the development of the third-generation semiconductor industry, and silicon carbide power devices can effectively meet the requirements of high efficiency, miniaturization and light weight of power electronic systems due to excellent performances of high pressure resistance, high temperature resistance, low loss and the like. The method has obvious advantages in the fields of new energy automobiles, photovoltaic power generation, rail transit, smart power grids and the like.
Since extremely small amount of metal contamination on the surface of the silicon carbide epitaxial wafer may cause device function failure or poor reliability, metal impurity control of the silicon carbide epitaxial wafer during the manufacturing and use process is very important.
At present, the method for detecting the trace metal elements on the surface of the silicon carbide epitaxial wafer has no related documents and standards, and the invention provides a method for determining the trace metal elements on the surface of the silicon carbide epitaxial wafer aiming at the technical blank, so that the method is rapid and reliable, and has high precision and accuracy.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide the method for detecting the trace metals on the surface of the silicon carbide epitaxial wafer, the quantitative analysis of various metal elements on the surface of the silicon carbide epitaxial wafer can be rapidly and accurately carried out by utilizing the method, and the quality of the silicon carbide wafer is ensured to be controllable.
In order to achieve the purpose, the invention provides a method for detecting trace metals on the surface of a silicon carbide epitaxial wafer, which comprises the following steps:
s1, adjusting an inductively coupled plasma mass spectrometer by using tuning liquid, and optimizing and tuning the working conditions and various parameters of the instrument to achieve the optimal test conditions;
step S2, diluting the standard sample: diluting the diluted standard sample solution into mixed standard solutions with different concentrations by using a clean volumetric flask and an analytical balance; the concentration gradient of each element is 0.00 mu g/L,0.10 mu g/L,0.20 mu g/L,0.50 mu g/L,1.00 mu g/L and 2.00 mu g/L;
s3, drawing a standard curve; inserting sample tubes of the inductively coupled plasma mass spectrometer into the standard series of measurement standard curve points of each concentration in sequence according to the working conditions of the instrument in the step S1, taking the average value of the three readings to calculate a standard curve, and drawing the standard curve by taking the signal of the element to be measured as a Y axis and the concentration of the standard substance as an X axis;
s4, preparing a scanning solution; sucking the back of the silicon carbide wafer by using a nonmetal vacuum suction pen, flatly placing the wafer, uniformly dripping 5ml of extracting solution on the center of the surface of the wafer by using a liquid transfer gun, slightly shaking the wrist to enable the solution to comprehensively and uniformly cover the whole surface of the wafer, staying for a moment, collecting the scanning solution into a PFA sample bottle, and performing on-machine test;
s5, measuring; on an inductively coupled plasma mass spectrometer, the scanning solution is tested according to the mass number of each metal element to be tested, the instrument automatically processes data according to a standard curve, and calculates and outputs the mass concentration of each element to be tested in the scanning solution.
Preferably, the extracting solution is a mixed solution of nitric acid and ultrapure water, wherein the volume fraction of the nitric acid is 2-8%.
Preferably, the resistivity of the ultrapure water is more than 18.0m Ω · cm; the mass fraction of the nitric acid added into the ultrapure water is between 68.0 and 70.0 percent, and the content of each metal element to be detected is less than 10ng/L.
Preferably, the diluted standard sample solution is a mixed element standard solution diluted to 200 μ g/L with ultrapure water, the mixed element standard solution: the method adopts a certified standard substance which can trace the source by quantity value, the mixed element standard substance contains all metal elements to be detected, and the mass concentration of the elements is 10mg/L.
Preferably, the mass concentration of beryllium, cerium, indium, lithium and uranium in the tuning liquid is 1 mug/L.
Preferably, the metal elements to be measured are: k, ca, na, al, ti, V, cr, mn, co, ni, cu, zn, W.
Preferably, the test temperature of the inductively coupled plasma mass spectrometer is 22 +/-2 ℃, and the test humidity is 35-50%.
Preferably, in the sample preparation and detection links, the requirement on the environment is to have 1000-grade ultra-clean room.
Preferably, all the test containers are soaked and washed by nitric acid, soaked and cleaned by ultrapure water of 18.0M omega cm, and dried by nitrogen.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention successfully establishes the method for detecting the content of 13 impurity metal elements on the surface of the silicon carbide epitaxial wafer, can accurately determine the content of the impurity metal elements on the surface of the silicon carbide epitaxial wafer by using the experimental conditions listed in the invention content, solves the problem of determination of the content of the impurity metal elements on the surface of the silicon carbide epitaxial wafer which is urgently needed in production, and meets the requirement of detection of the content of the impurity metal elements on the surface of the silicon carbide epitaxial wafer.
2. The method can be used for rapidly and accurately carrying out quantitative analysis on various metal elements on the surface of the silicon carbide epitaxial wafer and ensuring that the quality of the silicon carbide wafer is controllable.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are one embodiment of the present invention, and not all embodiments. All other embodiments obtained by a person skilled in the art based on the embodiments of the present invention without any creative work belong to the protection scope of the present invention.
The present invention provides a method for detecting trace metals on the surface of a silicon carbide epitaxial wafer, and the present invention is described in detail with reference to specific embodiments.
The principle of the detection method of the present invention is as follows: the inductively coupled plasma mass spectrometer (ICP-MS) has obvious advantages in the aspects of multi-element simultaneous analysis, analysis speed, detection limit and the like, can sensitively and reliably detect trace metal pollutants on the surface of a wafer,
the working principle is as follows: the method comprises the steps of collecting metal elements on the surface of a silicon carbide epitaxial wafer by using a nitric acid solution, introducing collected liquid into a high-temperature plasma source through an ICP-MS sample introduction system by using carrier gas, and carrying out desolventizing, evaporation, dissociation, atomization and ionization to form univalent positive ions. The ions enter a high-vacuum mass spectrum system through a three-cone interface system, and ion beams are introduced into the mass spectrum system through pressure difference and are deflected, focused and the like under the action of various ion lenses. The ion beam reaches the collision reaction tank, and different gases are introduced into the collision reaction tank to achieve the purpose of eliminating interference. Finally, the main quadrupole is reached, screening is carried out according to the mass-to-charge ratio (m/z) of ions, only the concerned elements are allowed to pass through, and the qualitative effect is achieved. And finally, the ion beam with the single mass-to-charge ratio (m/z) reaches a detector, is converted into an electric signal, is subjected to element quantification according to the signal intensity, obtains the mass concentration of the metal element to be detected, and further calculates the content of the metal element on the surface of the wafer.
1. Used experimental instrument
Inductively coupled plasma mass spectrometry (ICP-MS), a non-metal vacuum pipette, a PFA sample bottle, and a thousandth electronic analytical balance.
2. Reagent materials for experiments
2.1 nitric acid: 68.0-70.0% of mass fraction, and the content of each metal element to be detected is less than 10ng/L;
2.2 ultrapure water: the resistivity is more than 18.0m omega cm;
2.3 mixing element standard solution: adopting a certified standard substance which can trace the source by quantity value, wherein the mixed element standard substance comprises all metal elements to be detected, and the mass concentration of the elements is 10mg/L;
2.4 dilution of standard sample solution: diluting the mixed element standard solution to 200 mug/L by using ultrapure water;
2.5 extracting solution: a mixed solution of nitric acid and ultrapure water, wherein the volume fraction of the nitric acid is 2-8%;
2.6 tuning liquid: the mass concentration of beryllium, cerium, indium, lithium and uranium elements is 1 mu g/L.
3. Requirements of Experimental tests
3.1 the testing temperature and the testing humidity of the inductively coupled plasma mass spectrometer are respectively 22 +/-2 ℃ and 35-50%;
3.2 in the sample preparation and detection links, the method has very high requirements on the environment and has a 1000-level ultra-clean room;
3.3 the used experimental containers are soaked and washed by nitric acid, then soaked and cleaned by ultrapure water of 18.0M omega cm, and finally dried by nitrogen.
4. Test procedure
4.1 Instrument preparation: the tuning liquid is used for adjusting the inductively coupled plasma mass spectrometer, the working condition and various parameters of the instrument are optimized and tuned, the optimal test condition and the optimal working state are achieved, and the sensitivity is good;
4.2 working parameters: cooling gas: 12-15L/min; auxiliary air flow rate: 1.0-1.2L/min; flow rate of atomizing gas: 0.8-1.2L/min; the cooling gas, the auxiliary gas and the atomizing gas are argon.
The selection of the mass number of each element to be tested is shown in table 1.
| Element name | Mass number | Element name | Mass number |
| Potassium salt | 39 K | Manganese (Mn) | 55 Mn |
| Calcium carbonate | 40 Ca | Cobalt | 59 Co |
| Sodium salt | 23 Na | Nickel (II) | 60 Ni |
| Aluminium | 27 Al | Copper (Cu) | 63 Cu |
| Titanium (Ti) | 48 Ti | Zinc | 66 Zn |
| Vanadium oxide | 51 V | Tungsten | 182 W |
| Cadmium (Cd) | 52 Cr |
TABLE 1
4.2, diluting the standard sample:
diluting the diluted standard sample solution into mixed standard solutions with different concentrations by using a clean volumetric flask and an analytical balance; the concentration gradient of each element is 0.00 mu g/L,0.10 mu g/L,0.20 mu g/L,0.50 mu g/L,1.00 mu g/L and 2.00 mu g/L;
4.3, drawing a standard curve; inserting sample tubes of the inductively coupled plasma mass spectrometer into the standard series determination standard curve points of each concentration in sequence according to the working conditions of the instrument in the step S1, taking the average value of the three readings to calculate a standard curve, and drawing the standard curve by taking the element signal to be measured as a Y axis and the concentration of the standard substance as an X axis;
4.4, preparing a scanning solution; sucking the back of the silicon carbide wafer by using a nonmetal vacuum suction pen, flatly placing the wafer, uniformly dripping 5ml of extracting solution on the center of the surface of the wafer by using a liquid transfer gun, slightly shaking the wrist to enable the solution to comprehensively and uniformly cover the whole surface of the wafer, staying for a moment, collecting the scanning solution into a PFA sample bottle, and performing on-machine test;
4.5, measuring; on an inductively coupled plasma mass spectrometer, the scanning solution is tested according to the mass number of each metal element to be tested, the instrument automatically processes data according to a standard curve, and the mass concentration of each element to be tested in the scanning solution is calculated and output.
5. Data processing
The standard curve equation and detection limit of each metal element are shown in table 2:
| element(s) | Equation of standard curve | Correlation coefficient | Detection limit (ng/L) |
| K | Y＝9x-106 | 0.999969 | 0.858301 |
| Ca | Y＝3x+137 | 0.999711 | 5.534008 |
| Na | Y＝3x+9 | 0.999994 | 2.08587 |
| Al | Y＝1x-17 | 0.999918 | 3.877565 |
| Ti | Y＝4x+12 | 0.999998 | 1.925071 |
| V | Y＝7x-1 | 0.999999 | 0.063577 |
| Cr | Y＝8x+0 | 0.999996 | 0.677931 |
| Mn | Y＝8x+26 | 0.999971 | 1.795624 |
| Co | Y＝15x-49 | 0.999998 | 0.201565 |
| Ni | Y＝4x+9 | 0.999986 | 7.469195 |
| Cu | Y＝10x+29 | 0.999996 | 0.541408 |
| Zn | Y＝1x-18 | 0.999936 | 5.722373 |
| W | Y＝15x-15 | 0.999996 | 0.058192 |
TABLE 2
The method can be used for rapidly and accurately carrying out quantitative analysis on 13 metal elements on the surface of the silicon carbide wafer, wherein the 13 elements are as follows: k, ca, na, al, ti, V, cr, mn, co, ni, cu, zn, W; the method has the advantages of simple operation, high repeatability, low instrument detection limit and high precision.
The standard recovery test for the 1ppb standard solution was carried out using the test methods described above, and the results are shown in Table 3:
| element(s) | K | Ca | Na | Al | Ti |
| Recovery (%) | 98.14 | 101.41 | 99.16 | 101.57 | 101.17 |
| Element(s) | V | Cr | Mn | Co | Ni |
| Recovery (%) | 101.82 | 101.18 | 99.82 | 100.07 | 100.14 |
| Element(s) | Cu | Zn | W | ||
| Recovery (%) | 99.88 | 101.29 | 100.00 |
TABLE 3
As can be seen from the above table, the average recovery rate of the method is between 98% and 102%.
The invention uses the inductively coupled plasma mass spectrometer for testing, has low detection limit of the instrument, is in ppq-ppt level, has less interference, and can meet the requirement of measuring trace metal elements.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (9)
1. A method for detecting trace metals on the surface of a silicon carbide epitaxial wafer is characterized by comprising the following steps: the method comprises the following steps:
s1, adjusting an inductively coupled plasma mass spectrometer by using tuning liquid, optimizing and tuning the working conditions and various parameters of the instrument to achieve the optimal test conditions;
step S2, diluting the standard sample: diluting the diluted standard sample solution into mixed standard solutions with different concentrations by using a clean volumetric flask and an analytical balance; the concentration gradient of each element is 0.00 mu g/L,0.10 mu g/L,0.20 mu g/L,0.50 mu g/L,1.00 mu g/L and 2.00 mu g/L;
s3, drawing a standard curve; inserting sample tubes of the inductively coupled plasma mass spectrometer into the standard series determination standard curve points of each concentration in sequence according to the working conditions of the instrument in the step S1, taking the average value of the three readings to calculate a standard curve, and drawing the standard curve by taking the element signal to be measured as a Y axis and the concentration of the standard substance as an X axis;
s4, preparing a scanning solution; sucking the back of the silicon carbide wafer by using a nonmetal vacuum suction pen, flatly placing the wafer, uniformly dripping 5ml of extracting solution on the center of the surface of the wafer by using a liquid transfer gun, slightly shaking the wrist to enable the solution to comprehensively and uniformly cover the whole surface of the wafer, staying for a moment, collecting the scanning solution into a PFA sample bottle, and performing on-machine test;
s5, measuring; on an inductively coupled plasma mass spectrometer, the scanning solution is tested according to the mass number of each metal element to be tested, the instrument automatically processes data according to a standard curve, and calculates and outputs the mass concentration of each element to be tested in the scanning solution.
2. A method for detecting trace metals on the surface of silicon carbide epitaxial wafers as claimed in claim 1, wherein: the extracting solution is a mixed solution of nitric acid and ultrapure water, wherein the volume fraction of the nitric acid is 2-8%.
3. A method for detecting trace metals on the surface of silicon carbide epitaxial wafers as claimed in claim 2, wherein: the resistivity of the ultrapure water is more than 18.0m omega cm; the mass fraction of the nitric acid added into the ultrapure water is between 68.0 and 70.0 percent, and the content of each metal element to be detected is less than 10ng/L.
4. A method for detecting trace metals on the surface of silicon carbide epitaxial wafers as claimed in claim 1, wherein: the diluted standard sample solution is prepared by diluting a mixed element standard solution to 200 mu g/L with ultrapure water, wherein the mixed element standard solution comprises the following components in percentage by mass: the method adopts a certified standard substance which can trace the source by quantity value, the mixed element standard substance contains all metal elements to be detected, and the mass concentration of the elements is 10mg/L.
5. A method for detecting trace metals on the surface of silicon carbide epitaxial wafers as claimed in claim 1, wherein: the mass concentrations of beryllium, cerium, indium, lithium and uranium elements in the tuning liquid are all 1 mu g/L.
6. A method for detecting trace metals on the surface of silicon carbide epitaxial wafers as claimed in claim 1, wherein: the metal elements to be detected are as follows: k, ca, na, al, ti, V, cr, mn, co, ni, cu, zn, W.
7. A method for detecting trace metals on the surface of silicon carbide epitaxial wafers as claimed in claim 1, wherein: the testing temperature of the inductively coupled plasma mass spectrometer is 22 +/-2 ℃, and the testing humidity is 35-50%.
8. A method for detecting trace metals on the surface of silicon carbide epitaxial wafers as claimed in claim 1, wherein: in the sample preparation and detection links, the requirement on the environment is that 1000-grade ultra-clean room is required.
9. A method for detecting trace metals on the surface of silicon carbide epitaxial wafers as claimed in claim 1, wherein: all experimental containers are soaked and washed by nitric acid, soaked and cleaned by ultrapure water of 18.0M omega cm, and dried by nitrogen.
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