CN102539357A - Method for testing aluminum element content in aluminum gallium and nitrogen wafer epitaxial layer - Google Patents
Method for testing aluminum element content in aluminum gallium and nitrogen wafer epitaxial layer Download PDFInfo
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- CN102539357A CN102539357A CN2011104477177A CN201110447717A CN102539357A CN 102539357 A CN102539357 A CN 102539357A CN 2011104477177 A CN2011104477177 A CN 2011104477177A CN 201110447717 A CN201110447717 A CN 201110447717A CN 102539357 A CN102539357 A CN 102539357A
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- aluminium element
- aluminum gallium
- etching
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Abstract
The invention belongs to the technical field of metering test and relates to the technical field of chemical ingredient content test. The invention relates to a method for testing the aluminum element content in an aluminum gallium and nitrogen wafer epitaxial layer. A molten sodium hydroxide is adopted for etching the aluminum gallium and nitrogen wafer epitaxial layer for many times, etched samples are neutralized by hydrochloric acid, strong acid solution of aluminum elements is formed, the spectrophotometry is adopted for measuring the absorbance of the aluminum element of the etching liquid and chromazurine S color developing solution at a 546nm position, the aluminum element concentration of the sample solution can be obtained through the relationship between the standard solution absorbance and the aluminum element concentration, then, the aluminum content in the wafer epitaxial layer can be obtained according to the measured aluminum element concentration, and a deep ultraviolet photoluminescence spectrometer is adopted for measuring the etching surface fluorescence peak occurrence position to control the etching depth. The repeated measurement deviation is about 1 percent, and the standard recovery rate is higher than 95 percent. The method is applicable to the accurate test of the aluminum element content in the aluminum gallium and nitrogen wafer epitaxial layer.
Description
One, affiliated technical field
The invention belongs to the metrological testing technology field, relate to the chemical constitution quantitative analysis tech, particularly aluminium element quantitative test technique in the aluminum gallium nitride crystal.
Two, background technology
Aluminum gallium nitride (
) is the important materials of preparation deep ultraviolet detector; The aluminum gallium nitride wafer is usually by metal organic chemical vapor deposition (mocvd) method or molecular beam epitaxy preparation; The energy gap of aluminium element content and material is closely related in the wafer epitaxial loayer; Be an important indicator of decision aluminum gallium nitride ultraviolet detector response wave band, the content of accurately measuring aluminium element in the aluminum gallium nitride wafer epitaxial loayer has realistic meaning for the research of Al-Ga-N material.Because the several at the most micron of aluminum gallium nitride wafer epitaxy layer thickness, accurately test in the epitaxial loayer relatively difficulty of aluminium element content.The method of aluminium element is physical methods such as UV, visible light optical transmission method, high-resolution X-ray diffraction method, Rutherford backscattering method in the testing wafer epitaxial loayer at present; The physics method is just through measuring the physical parameter relevant with aluminium element content; Go out the content of aluminium element then through the calculated with mathematical model of aluminium element content and physical parameter; Physics method measurement result receives the restriction of sample grown quality and mathematical model, and the uncertainty source of measurement result is indeterminate.
The UV, visible light optical transmission method is through measuring the optical energy gap of wafer; Carry out quantitatively according to the theoretical formula of optical energy gap and aluminium element content; Owing to contain the bend factor b of Al-Ga-N material in the computing formula; And bibliographical information is inconsistent, therefore adopts the UV, visible light optical transmission method can't obtain the exact value of aluminium element.
The high-resolution X-ray diffraction method is through accurately recording the grating constant of aluminum gallium nitride crystal, calculating aluminium element content according to Wei Jiade theorem (the linear corresponding relation of grating constant and material component).Because the method is had relatively high expectations to material, only is applicable to the ideal crystal of no strain or the complete relaxation of strain, therefore can there be bigger error in the result of calculation to the aluminum gallium nitride wafer.
The Rutherford backscattering method is the easy reliable and nondestructive method of analysed film sample; Usually adopt SIMNRA or RUMP program that the backward scattering random spectrum of a certain crystallographic axis of extension membrane material is simulated; Can obtain the stoichiometric proportion of each element in the sample; The method is for the quantitative poor accuracy of nitrogen element, and domestic existing proving installation is few in number, and the source of error of method of testing and influence factor are not clear and definite as yet yet.
The report that does not also have the chemical analysis aspect of aluminium element content in the relevant aluminum gallium nitride wafer epitaxial loayer at present both at home and abroad.
Three, summary of the invention
The present invention is intended to being grown in the aluminum gallium nitride crystal epitaxial layer on the backing material a kind of chemical analysis of aluminium element content is provided.
The purpose of patent of the present invention is achieved in that the aluminum gallium nitride in the NaOH etching epitaxial loayer that adopts fusion, and molten sodium hydroxide and aluminum gallium nitride reaction generate sodium metaaluminate;
Al
xGa
1-xN+NaOH→NaAlO
2+Ga
2O
3+NH
3↑
Then the sodium hydroxide solution that etches away with excessive hydrochloric acid (6molL
-1) neutralization, solution need keep highly acid, the pH=2 of solution～3, and this moment, following reaction took place in aluminium element, had generated AlCl
3:
NaAlO
2+HCl→AlCl
3+NaCl+H
2O
With hydrochloric acid and ammoniacal liquor to containing AlCl
3Solution carry out acidity adjustment, adopting chrome azurol S is complexing colour developing body, chrome azurol S and Al
3+Complex reaction takes place; The chromophoric solution medium is the acetate sodium acetate buffer solution; Adopt the absorbance at spectrophotometer measurement solution 546nm place; Draw aluminium element content and absorbance typical curve according to the absorbance that adds aluminum standard solution and chrome azurol S complexing chromophoric solution, the absorbance according to etching liquid can calculate the aluminium element quality in the etching liquid again.
Adopt deep ultraviolet photoluminescence spectroscopy control etching degree, improve the effective rate of transform of sample, the error of avoiding overetch to introduce, thus improve measuring accuracy.
The method of testing of aluminium element content comprises sample preparation in the aluminum gallium nitride wafer epitaxial loayer that the present invention relates to, and epitaxial loayer etching, chemical complexing, absorbance test and comparison, calculating convert and obtains aluminium element content,
(1) sample pretreatment: soak sample with watery hydrochloric acid and remove water-solubility impurity, washed with de-ionized water is soaked oil removing with analyzing pure acetone, drying, accurately weighing (being accurate to 0.001mg) to neutral;
(2) etching: at the Powdered NaOH of print surface tiling skim, be heated to the complete fusion of NaOH, the NaOH that insulation is etched to fusion is transparent fully, and cooling with deionized water dissolving etching thing, obtains etching liquid;
Regulate etching liquid acidity pH value between 2～3 with hydrochloric acid, constant volume obtains testing sample;
(3) aluminum standard solution preparation
With strong caustic heating for dissolving rafifinal, between 2～3, constant volume obtains the aluminium element standard solution with hydrochloric acid conditioning solution pH value;
(4) complexing colour developing: making indicator with thymol blue, is complexing agent with the chrome azurol S; In acetate-sodium acetate buffer system, be blush with hydrochloric acid and the ammoniacal liquor system of transferring to, obtain the absorbance test solution;
(5) absorbance test and data processing
Test complexing colour developing aluminum standard solution is drawn aluminium element content and absorbance and is concerned typical curve in the absorbance of 546 ± 5nm; With the absorbance of testing sample absorbance solution,, be calculated as follows and obtain in the sample aluminium element content in the aluminum gallium nitride wafer epitaxial loayer with typical curve comparison at the 546nm place:
In the formula: w
AlAluminium element massfraction in the-aluminum gallium nitride epitaxial loayer;
The quality of the aluminium element that m-metric measurement obtains;
m
0The original quality of-aluminum gallium nitride wafer;
m
1The quality of aluminum gallium nitride wafer after the-etching.
The method of testing of aluminium element content in the aluminum gallium nitride wafer epitaxial loayer that the present invention relates to, said sample etching process is a multiple etching.
The method of testing of aluminium element content in the aluminum gallium nitride wafer epitaxial loayer that the present invention relates to, said sample etching process single sodium hydroxide concentration is not more than 0.05g/cm
2
The method of testing of aluminium element content in the aluminum gallium nitride wafer epitaxial loayer that the present invention relates to, said sample etching process single sodium hydroxide concentration is not more than 0.02g/cm
2
The method of testing of aluminium element content in the aluminum gallium nitride wafer epitaxial loayer that the present invention relates to; Said sample etching degree adopts the deep ultraviolet photoluminescence spectroscopy; Measure wavelength between 230～350nm; Measure step-length≤10nm, with 3300
near to go out the peak be etching terminal.
The method of testing of aluminium element content in the aluminum gallium nitride wafer epitaxial loayer that the present invention relates to; Said sample etching degree adopts the deep ultraviolet photoluminescence spectroscopy; Measure wavelength between 230～350nm; Measure step-length between 3～10nm, with 3300
near to go out the peak be etching terminal.
The method of testing of aluminium element content in the aluminum gallium nitride wafer epitaxial loayer that the present invention relates to, said adjusting acidity with the concentration of hydrochloric acid between 0.6～6.0molL
-1Between.
The method of testing of aluminium element content in the aluminum gallium nitride wafer epitaxial loayer that the present invention relates to, said adjusting acidity is used the combined system of ammoniacal liquor as the ammoniacal liquor of variable concentrations.
The method of testing of aluminium element content in the aluminum gallium nitride wafer epitaxial loayer that the present invention relates to, said adjusting acidity uses ammoniacal liquor to be 2molL
-1And 0.1molL
-1Combined system.
The method of testing of aluminium element content in the aluminum gallium nitride wafer epitaxial loayer that the present invention relates to, the aluminium element content of said aluminum standard solution is between 5～20 μ gml
-1Between.
Aluminium element content test method in the aluminum gallium nitride wafer epitaxial loayer of the present invention; The standard deviation of duplicate measurements is approximately 1%; Recovery of standard addition is greater than 95%; Be applicable to the accurate test of aluminium element content in the aluminum gallium nitride wafer epitaxial loayer; The physics methods such as Rutherford backscattering method, high-resolution X-ray diffraction method that can be used as are measured a kind of verification method of aluminium element content in the aluminum gallium nitride wafers, also can be used as a kind of valued methods of aluminum gallium nitride epitaxial wafer ingredient standard substance, have realistic meaning for the relation of aluminium element content and its photoelectric properties in the research wafer.
Description of drawings
Accompanying drawing 1 is the fluorescence peak of epitaxial film materials when not etching into substrate;
Accompanying drawing 2 is the fluorescence peak of the epitaxial material of etching during near substrate and the fluorescence peak of backing material;
Accompanying drawing 3 is chromophoric solution maximum absorption wavelengths.
Four, embodiment
Below in conjunction with embodiment sample processing and the method for testing that the present invention relates to is described in detail, but not as limitation of the present invention.
Embodiment one
(1) sample pretreatment
Getting an area is 5cm
2Square aluminum gallium nitride wafer, immerse to soak in 5% the watery hydrochloric acid and remove water-solubility impurity half an hour, to neutral, soak oil removing in ten minutes with washed with de-ionized water with analyzing pure acetone, drying accurately is weighed as 444.547mg (m
0).
(2) etching: lie in a horizontal plane in the aluminum gallium nitride sample wafer of handling well in the platinum crucible; Epitaxial loayer evenly is tiled in sample surfaces towards last with the Powdered analysis pure cerium hydroxide of 0.75g sodium, is heated to the complete fusion of NaOH; The NaOH that insulation is etched to fusion is transparent fully; Cooling is with deionized water dissolving etching thing, with obtaining etching liquid; Etching liquid is transferred in the 250ml volumetric flask, used 6molL
-1Hydrochloric acid regulation system pH reaches between 2～3, uses the deionized water constant volume, shakes up and obtains testing sample solution;
Clean also and be weighed as 443.941mg (m1) behind the dry print, the quality that then etches away epitaxial film is 0.606mg (m
0-m
1).
(3) aluminium element standard solution preparation
Take by weighing 24.163mg rafifinal (purity is greater than 99.999%) in the platinum crucible of cleaning, add 800mg and analyze pure cerium hydroxide sodium and 3ml deionized water, heating for dissolving aluminium, the cooling back moves into the 250ml volumetric flask, shakes up, and obtains aluminium content 96.652 μ gml
-1Solution;
Pipette the above-mentioned solution of 25ml in the 250ml volumetric flask, add 10ml hydrochloric acid (6molL
-1), use the deionization constant volume, shake up, obtain solution aluminium content 9.6652 μ gml
-1Aluminum standard solution.
(4) complexing colour developing sample preparation: get the 20ml etching liquid in the 100ml volumetric flask, drip the blue solution of 2 phenol, add 2ml hydrochloric acid (0.6molL successively
-1), 0.5ml ammoniacal liquor (2molL
-1), use 0.1molL
-1Ammoniacal liquor transfers to solution and is blush, adds 1.0ml hydrochloric acid (0.6 molL more successively
-1), 1.0ml ascorbic acid solution (20gL
-1), 2.0ml thiourea solution (100gL
-1), 2.5ml chrome azurol S solution (2gL
-1) and 5ml acetate-sodium acetate buffer solution, a kind of reagent of every adding all need shake up, and is diluted with water to scale, shakes up, and obtains complexing colour developing sample to be measured.
(4) complexing aluminum standard solution preparation: pipette the aluminum standard solution that 0 (blank), 1.0,2.0,3.0,4.0,5.0ml prepare and place one group of (6) 100ml volumetric flask respectively; Add deionized water to about 10ml; Step preparation standard complexing colour developing sample by (4) obtains one group of (6) standard complexing colour developing aluminium standard model.
(5) absorbance test and data processing: leave standstill 15min after the sample complexing colour developing; With the reagent blank is reference, with the absorbance of each sample of spectrophotometer test 546nm place, is horizontal ordinate with the absorbance; Adding the aluminum standard solution volume is ordinate drawing curve; Shown in accompanying drawing 1, the typical curve fit equation is V=5.448A+0.30689, and coefficient R is 0.99816; The absorbance of complexing to be measured colour developing sample (etching liquid) is 0.358, and with the typical curve comparison and calculate that contained aluminium element gross mass is 272.930 μ g in the etching liquid, the massfraction that calculates aluminium element in the AlGaN epitaxial film by formula (1) is 45.04%.
Pipette 20ml etching liquid and 1ml aluminum standard solution simultaneously in the 100ml volumetric flask, process above repeating, preparation adds target complexing chromophoric solution.The absorbance of mark-on complexing chromophoric solution is 0.534, and recovery of standard addition is 95.88%.
Embodiment two
Get an area 4cm
2(sample identical) with embodiment one, weight 357.63mg, sample preparation adopts multiple etching, and all the other processing procedure processes are with embodiment one.
Etching is used the Powdered analysis pure cerium hydroxide of 0.2g sodium for the first time, with DUV photoluminescence spectrometer measurement, tests wavelength 235nm behind the sample drying, step-length 10, and fluorescence peak is shown in accompanying drawing 2.
Carry out the etching second time with the Powdered analysis pure cerium hydroxide of 0.2g sodium, with DUV photoluminescence spectrometer measurement, test wavelength 235nm behind the sample drying, step-length 10, fluorescence peak is shown in accompanying drawing 2.
Carry out etching for the third time with the Powdered analysis pure cerium hydroxide of 0.2g sodium, with DUV photoluminescence spectrometer measurement, test wavelength 235nm behind the sample drying, step-length 10, fluorescence peak reaches etching terminal shown in accompanying drawing 3.
Preceding twice etching liquid merging is tested and calculated, and the massfraction that obtains aluminium element in the AlGaN epitaxial film is 45.60%.
Multiple etching and single etching measurement result have consistance, and standard deviation is 0.4%.
Claims (10)
1. the method for testing of aluminium element content in the aluminum gallium nitride wafer epitaxial loayer comprises sample preparation, epitaxial loayer etching, chemical complexing, absorbance test and comparison, calculates to convert and obtains aluminium element content, comprising:
(1) sample pretreatment: soak sample with watery hydrochloric acid and remove water-solubility impurity, washed with de-ionized water is soaked oil removing with analyzing pure acetone, drying, accurately weighing (being accurate to 0.001mg) to neutral;
(2) etching: at the Powdered NaOH of print surface tiling skim, be heated to the complete fusion of NaOH, the NaOH that insulation is etched to fusion is transparent fully, and cooling with deionized water dissolving etching thing, obtains etching liquid;
Regulate etching liquid acidity pH value between 2～3 with hydrochloric acid, constant volume obtains testing sample;
(3) aluminum standard solution preparation
With strong caustic heating for dissolving rafifinal, between 2～3, constant volume obtains the aluminium element standard solution with the hydrochloric acid conditioning solution pH value;
(4) complexing colour developing: making indicator with thymol blue, is complexing agent with the chrome azurol S; In acetate-sodium acetate buffer system, be blush with hydrochloric acid and the ammoniacal liquor system of transferring to, obtain the absorbance test solution;
(5) absorbance test and data processing
Test complexing colour developing aluminum standard solution is 546
± 5The absorbance of nm is drawn aluminium element content and absorbance and is concerned typical curve; With the absorbance of testing sample absorbance solution,, be calculated as follows and obtain in the sample aluminium element content in the aluminum gallium nitride wafer epitaxial loayer with typical curve comparison at the 546nm place:
In the formula: w
AlAluminium element massfraction in the-aluminum gallium nitride epitaxial loayer;
The quality of the aluminium element that m-metric measurement obtains;
m
0The original quality of-aluminum gallium nitride wafer;
m
1The quality of aluminum gallium nitride wafer after the-etching.
2. the method for testing of aluminium element content in the aluminum gallium nitride wafer epitaxial loayer that relates to of claim 1, said sample etching process is a multiple etching.
3. the method for testing of aluminium element content in the aluminum gallium nitride wafer epitaxial loayer that relates to of claim 2, said sample etching process single sodium hydroxide concentration is not more than 0.05g/cm2.
4. the method for testing of aluminium element content in the aluminum gallium nitride wafer epitaxial loayer that relates to of claim 2, said sample etching process single sodium hydroxide concentration is not more than 0.02g/cm2.
5. the method for testing of aluminium element content in the aluminum gallium nitride wafer epitaxial loayer that relates to of claim 1; Said sample etching degree adopts the deep ultraviolet photoluminescence spectroscopy; Measure wavelength between 230～350nm; Measure step-length≤10nm, with 3300
near to go out the peak be etching terminal.
6. the method for testing of aluminium element content in the aluminum gallium nitride wafer epitaxial loayer that relates to of claim 5; Said sample etching degree adopts the deep ultraviolet photoluminescence spectroscopy; Measure wavelength between 230～350nm; Measure step-length between 3～10nm, with 3300
near to go out the peak be etching terminal.
7. the method for testing of aluminium element content in arbitrary aluminum gallium nitride wafer epitaxial loayer of relating to of claim 1～6, said adjusting acidity with the concentration of hydrochloric acid between 0.6～6.0 molL-1.
8. the method for testing of aluminium element content in arbitrary aluminum gallium nitride wafer epitaxial loayer of relating to of claim 1～6, said adjusting acidity is used the combined system of ammoniacal liquor as the ammoniacal liquor of variable concentrations.
9. the method for testing of aluminium element content in the aluminum gallium nitride wafer epitaxial loayer that relates to of claim 8, it is the combined system of 2 molL-1 and 0.1 molL-1 that said adjusting acidity is used ammoniacal liquor.
10. the method for testing of aluminium element content in arbitrary aluminum gallium nitride wafer epitaxial loayer of relating to of claim 1～6, the aluminium element content of said aluminum standard solution is between 5～20 μ gml-1.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103196850A (en) * | 2013-04-03 | 2013-07-10 | 中国兵器工业集团第五三研究所 | Method for testing indium content in epitaxial layer of InGaN chip |
| CN105973880A (en) * | 2016-04-25 | 2016-09-28 | 天津科技大学 | Ready-to-use test paper for rapid assessment of content of aluminum elements in food, and use method and application thereof |
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| CN1619289A (en) * | 2003-11-21 | 2005-05-25 | 兰州理工大学 | Detecting method of aluminium and aluminium alloy oxide impuring content |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103196850A (en) * | 2013-04-03 | 2013-07-10 | 中国兵器工业集团第五三研究所 | Method for testing indium content in epitaxial layer of InGaN chip |
| CN105973880A (en) * | 2016-04-25 | 2016-09-28 | 天津科技大学 | Ready-to-use test paper for rapid assessment of content of aluminum elements in food, and use method and application thereof |
| CN105973880B (en) * | 2016-04-25 | 2019-02-12 | 天津科技大学 | The instant test paper and its application method of a kind of rapid evaluation aluminum in food constituent content and application |
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