CN101381893B - CdGeAs2 crystal etching agent and etching method - Google Patents
CdGeAs2 crystal etching agent and etching method Download PDFInfo
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- CN101381893B CN101381893B CN2008100462861A CN200810046286A CN101381893B CN 101381893 B CN101381893 B CN 101381893B CN 2008100462861 A CN2008100462861 A CN 2008100462861A CN 200810046286 A CN200810046286 A CN 200810046286A CN 101381893 B CN101381893 B CN 101381893B
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- hydrochloric acid
- nitric acid
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Abstract
The invention provides a corrosive agent for a CdGeAs2 crystal, which is prepared from hydrochloric acid, nitric acid and pure water, wherein the volume ratio of the hydrochloric acid to the nitric acid to the pure water is 1 to 1 to 1, the mass concentration of the hydrochloric acid is between 35 and 38 percent, and the mass concentration of the nitric acid is between 65 and 68 percent. A CdGeAs2 crystal corrosion method utilizing the corrosive agent orderly comprises the following processing: (1) a step of corrosion, in which a CdGeAs2 crystal wafer is subjected to grinding and polishing and is immersed in the corrosive agent, is corroded by swinging at normal pressure and at a temperature of between 15 and 30 DEG C for 15 to 40 seconds and is taken out; (2) a step of washing, in which the CdGeAs2 crystal wafer taken out of the corrosive agent is immersed in an alkaline cleaner to stop the corrosive reaction, and is washed to be neutral by pure water; and (3) a step of drying, in which the washed CdGeAs2 crystal wafer is naturally dried or oven-dried at the normal pressure.
Description
Technical field
The invention belongs to the corrosion field of ternary semiconductor material, particularly a kind of CdGeAs
2Crystal corrosive and caustic solution.
Background technology
Chalcopyrite crystalloid CdGeAs
2(being called for short CGA), belong to tetragonal, point group I42d is a kind of infrared non-linear optical material.CdGeAs
2The warm coefficient of expansion of crystal heat differs more than 15 times along a axle and c axle, makes that the growth of complete nothing cracking crystalline is very difficult, and the crystal that grows out exists numerous defectives.What of various generation of defects and quantity are not only relevant with crystal preparation technology, and the performance to fabricate devices has material impact simultaneously.
The experimental observation method of lattice defect has multiple, as methods such as transmission electron microscope, scanning electronic microscope, infrared microscope and etching pit demonstrations.Wherein, etching pit explicit representation and scanning electronic microscope are one of the most frequently used methods of observational study lattice defect, and not only equipment is simple, and is easy and simple to handle, and can show crystallographic direction more intuitively, aspect definite crystal indices and crystalline orientation, used by wide model.Etching pit shows quantity and the distribution situation can also disclose defective, finds out the relation of defective formation, propagation and crystal preparation technology and device technology, is to improve technology, reduces defective, improves the device qualification rate and improve device performance and give a clue.
CdGeAs
2Crystalline etching pit, especially preferential etch are technical barriers.At present, to CdGeAs
2The report of Robert S.Feigelson group of Stanford Univ USA is only seen in the crystalline corrosion, and employed etching reagent is: HNO
3: HF:H
2O=1:1:2 (volume ratio), etching time are 10 minutes～14 minutes.But its viewed pit figure is clear inadequately, does not see the three-dimensional pit feature image of regular shape.In addition, about CdGeAs
2The crystalline corrosion research does not appear in the newspapers.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of CdGeAs of being used for is provided
2Agent of crystalline preferential etch and caustic solution are so that to CdGeAs
2Crystal carries out preferential etch, obtains this crystal corrosion pit pattern.
CdGeAs of the present invention
2Crystal corrosive is formulated by hydrochloric acid, nitric acid and pure water, and the volume ratio of hydrochloric acid, nitric acid, pure water is a hydrochloric acid: nitric acid: pure water=1:1:1, and the mass concentration of described hydrochloric acid is 35～38%, the mass concentration of described nitric acid is 65～68%.
The used pure water of above-mentioned etching reagent is deionized water or distilled water.
CdGeAs of the present invention
2The crystalline caustic solution uses above-mentioned etching reagent, and its processing step is as follows successively:
(1) corrosion
With the CdGeAs after grinding, the polished finish
2Wafer immerses in the etching reagent, takes out in 15 seconds～40 seconds in normal pressure, 15 ℃～30 ℃ corrosion under swing;
(2) clean
The CdGeAs that will from etching reagent, take out
2Wafer immerses in the alkaline cleaner and stops corrosion reaction (5 seconds～10 seconds time), cleans to neutral with pure water again;
(3) drying
With the CdGeAs after cleaning
2Wafer is seasoning or oven dry under normal pressure.
In the aforesaid method, alkaline cleaner is the NaOH solution of mass concentration 5～10% or the NaCO of mass concentration 10～20%
3The KOH solution of solution or mass concentration 5～10%.Pure water is deionized water or distilled water.If adopt the mode drying of oven dry, preferred 40 ℃～60 ℃ of bake out temperature, drying time was at least 2 hours.
The present invention has following beneficial effect:
1, experiment shows that etching reagent of the present invention and caustic solution are to CdGeAs
2Crystal has good preferential etch, the CdGeAs after the corrosion
2Wafer can clearly demonstrate the corrosion pit pattern of a certain crystal face under metaloscope.
2, the raw material of etching reagent of the present invention is a conventional chemical reagent, and cost is low, is easy to obtain.
3, caustic solution of the present invention carries out under normal pressure, room temperature, and the time is short, easy to operate.
4, by the CdGeAs after the caustic solution corrosion of the present invention
2The metallography microscope photo of wafer can calculate the dislocation desity of growing crystal, is the preliminary CdGeAs of judge
2The screening of crystal mass, wafer provides a kind of simple and easy to do method.
Description of drawings
Fig. 1 is to use etching reagent of the present invention and CdGeAs that caustic solution obtains
2The pit shape appearance figure of crystal (101) crystal face;
Fig. 2 is CdGeAs
2The multistage X-ray diffraction spectrum of crystal (101) crystal face;
Fig. 3 is to use etching reagent of the present invention and CdGeAs that caustic solution obtains
2The pit shape appearance figure of crystal (312) crystal face;
Fig. 4 is CdGeAs
2The X-ray diffraction spectrum of crystal (312) crystal face.
Embodiment
Embodiment 1
In the present embodiment, CdGeAs
2Crystal corrosive is formulated by hydrochloric acid, nitric acid and deionized water, and the mass concentration of described hydrochloric acid is 35～38%, and the mass concentration of described nitric acid is 65～68%.The volume ratio of hydrochloric acid, nitric acid, deionized water is a hydrochloric acid: nitric acid: deionized water=1:1:1, measure hydrochloric acid, nitric acid and deionized water respectively by described volume ratio, and then hydrochloric acid, nitric acid are added in the deionized water and stirs and promptly form etching reagent.
Embodiment 2
Present embodiment is to CdGeAs
2Crystalline (101) crystal face corrodes, and used etching reagent is the etching reagent of embodiment 1 preparation, and processing step is as follows successively:
(1) grinds and polishing
With CdGeAs
2It is that 0#-02#-04#-06# abrasive paper for metallograph of 50 μ m～5 μ m is roughly ground that crystal (101) wafer adopts average particle size distribution successively, fine grinding, the suspension liquid (mass ratio of white alundum powder and deionized water is 1:10) that re-uses white alundum powder (median size 0.5 μ m) and deionized water carried out mechanical polishing 20 minutes on silk, use deionized water rinsing then, obtain the CdGeAs of surfacing
2Wafer; Again the wafer after the mechanical polishing is placed the bromine methanol solution of mass concentration 3%, at room temperature soak and carry out chemical rightenning about 1 minute, use methyl alcohol, acetone, ethanol and washed with de-ionized water after the taking-up successively;
(2) corrosion
With the CdGeAs after grinding, the polished finish
2Crystal (101) wafer immerses in the etching reagent, takes out in 40 seconds in normal pressure, 15 ℃ of corrosion under swing;
(3) clean
The CdGeAs that will from etching reagent, take out
2Wafer immerses in the NaOH solution of mass concentration 5% swing and cleans and stop corrosion reaction, about 5 seconds of time, again with washed with de-ionized water to neutral;
(4) drying
With the CdGeAs after cleaning
2Wafer is put into baking oven, and in normal pressure, 40 ℃ of dry for standby, drying time is 4 hours.
With dried CdGeAs
2Wafer metallography microscope sem observation, the pattern of its corrosion pit as shown in Figure 1, as can be seen from Figure 1, the pit pattern is the consistent isosceles triangle of orientation, sharpness of border has stereoscopic sensation.
Embodiment 3
In the present embodiment, CdGeAs
2Crystal corrosive is formulated by hydrochloric acid, nitric acid and distilled water, and the mass concentration of described hydrochloric acid is 35～38%, and the mass concentration of described nitric acid is 65～68%.The volume ratio of hydrochloric acid, nitric acid, distilled water is a hydrochloric acid: nitric acid: distilled water=1:1:1, measure hydrochloric acid, nitric acid and distilled water respectively by described volume ratio, and then hydrochloric acid, nitric acid are added in the distilled water and stirs and promptly form etching reagent.
Embodiment 4
Present embodiment is to CdGeAs
2Crystalline (312) crystal face corrodes, and used etching reagent is the etching reagent of embodiment 3 preparations, and processing step is as follows successively:
(1) grinds and polishing
With CdGeAs
2It is that 0#-02#-04#-06# abrasive paper for metallograph of 50 μ m～5 μ m is roughly ground that crystal (312) wafer adopts average particle size distribution successively, fine grinding, white alundum powder (the median size 0.5 μ m) suspension liquid (mass ratio of white alundum powder and deionized water is 1:10) that re-uses the distilled water preparation carried out mechanical polishing 20 minutes on silk, use distilled water flushing then, obtain the CdGeAs of surfacing
2Wafer; Again the wafer after the mechanical polishing is placed the bromine methanol solution of mass concentration 3%, at room temperature soak and carry out chemical rightenning about 1 minute, clean with methyl alcohol, acetone, ethanol and distilled water successively after the taking-up;
(2) corrosion
With the CdGeAs after grinding, the polished finish
2Crystalline (312) wafer immerses in the etching reagent, takes out in 15 seconds in normal pressure, 30 ℃ of corrosion under swing;
(3) clean
The CdGeAs that will from etching reagent, take out
2Wafer immerses the NaCO of mass concentration 20%
3Swing is cleaned and is stopped corrosion reaction in the solution, about 10 seconds of time, cleans to neutral with distilled water again;
(4) drying
With the CdGeAs after cleaning
2Wafer is put into baking oven, and in normal pressure, 60 ℃ of dry for standby, drying time is 2 hours.
With dried CdGeAs
2Wafer metallography microscope sem observation, the pattern of its corrosion pit as shown in Figure 3, as can be seen from Figure 3, pit is the consistent square of orientation, sharpness of border has stereoscopic sensation.
Claims (7)
1. CdGeAs
2Crystal corrosive, it is characterized in that by hydrochloric acid, nitric acid and pure water formulated, the volume ratio of hydrochloric acid, nitric acid, pure water is a hydrochloric acid: nitric acid: pure water=1:1:1, and the mass concentration of described hydrochloric acid is 35～38%, the mass concentration of described nitric acid is 65～68%.
2. CdGeAs according to claim 1
2Crystal corrosive is characterized in that pure water is deionized water or distilled water.
3. CdGeAs
2The crystalline caustic solution is characterized in that processing step is as follows successively:
(1) corrosion
With the CdGeAs after grinding, the polished finish
2Wafer immerses in the etching reagent, under swing, took out in 15 seconds～40 seconds in normal pressure, 15 ℃～30 ℃ corrosion,
(2) clean
The CdGeAs that will from etching reagent, take out
2Wafer immerses in the alkaline cleaner and stops corrosion reaction, cleans to neutral with pure water again;
(3) drying
With the CdGeAs after cleaning
2Wafer is seasoning or oven dry under normal pressure;
Described etching reagent is formulated by hydrochloric acid, nitric acid and pure water, and the volume ratio of hydrochloric acid, nitric acid, pure water is a hydrochloric acid: nitric acid: pure water=1:1:1, and the mass concentration of described hydrochloric acid is 35～38%, the mass concentration of described nitric acid is 65～68%.
4. CdGeAs according to claim 3
2The crystalline caustic solution is characterized in that alkaline cleaner is the NaOH solution of mass concentration 5～10% or the NaCO of mass concentration 10～20%
3The KOH solution of solution or mass concentration 5～10%.
5. according to claim 3 or 4 described CdGeAs
2The crystalline caustic solution is characterized in that pure water is deionized water or distilled water.
6. according to claim 3 or 4 described CdGeAs
2The crystalline caustic solution is characterized in that the bake out temperature in the drying step is 40 ℃～60 ℃, and drying time was at least 2 hours.
7. CdGeAs according to claim 5
2The crystalline caustic solution is characterized in that the bake out temperature in the drying step is 40 ℃～60 ℃, and drying time was at least 2 hours.
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| CN2008100462861A CN101381893B (en) | 2008-10-16 | 2008-10-16 | CdGeAs2 crystal etching agent and etching method |
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| CN101381893B true CN101381893B (en) | 2010-09-29 |
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| CN101694012B (en) * | 2009-10-19 | 2011-09-21 | 中国电子科技集团公司第五十五研究所 | Wet etching method of barium-strontium titanate and bismuth zinc niobate composite films |
| CN105241885A (en) * | 2015-09-30 | 2016-01-13 | 金川集团股份有限公司 | Forged magnetically soft alloy 1J50 alloy metallographic corrosive liquid and applications thereof |
| CN105588746A (en) * | 2015-12-12 | 2016-05-18 | 中国航空工业标准件制造有限责任公司 | Corrosion agent and corrosion test method for displaying flow lines in high-temperature alloy heading state |
| CN106153659B (en) * | 2016-06-21 | 2019-01-25 | 四川大学 | CdSiP2The corrosive agent and caustic solution of crystal |
| CN109110810B (en) * | 2018-09-29 | 2020-09-01 | 中国电子科技集团公司第四十六研究所 | Steady flow synthesis method of arsenic germanium cadmium crystal growth raw material |
| CN112504724A (en) * | 2020-12-10 | 2021-03-16 | 北方民族大学 | Method for detecting c-plane growth dislocation density of sapphire wafer |
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