CN113718257A - Etching method of germanium ingot - Google Patents
Etching method of germanium ingot Download PDFInfo
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- CN113718257A CN113718257A CN202110980367.4A CN202110980367A CN113718257A CN 113718257 A CN113718257 A CN 113718257A CN 202110980367 A CN202110980367 A CN 202110980367A CN 113718257 A CN113718257 A CN 113718257A
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- Prior art keywords
- germanium
- acid
- germanium ingot
- etching
- ingot
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- 229910052732 germanium Inorganic materials 0.000 title claims abstract description 127
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 title claims abstract description 127
- 238000005530 etching Methods 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 32
- 239000002253 acid Substances 0.000 claims abstract description 80
- 238000005260 corrosion Methods 0.000 claims abstract description 46
- 230000007797 corrosion Effects 0.000 claims abstract description 46
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 42
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 38
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 35
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 21
- 239000007788 liquid Substances 0.000 claims abstract description 19
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 10
- 239000003517 fume Substances 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 238000004140 cleaning Methods 0.000 claims abstract description 5
- 239000008367 deionised water Substances 0.000 claims abstract description 5
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 5
- 238000011010 flushing procedure Methods 0.000 claims abstract description 5
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 3
- 230000000052 comparative effect Effects 0.000 description 14
- 239000012535 impurity Substances 0.000 description 7
- 239000000428 dust Substances 0.000 description 6
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000003749 cleanliness Effects 0.000 description 3
- 238000010790 dilution Methods 0.000 description 3
- 239000012895 dilution Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 238000007664 blowing Methods 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000000861 blow drying Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000004857 zone melting Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
- C23F1/30—Acidic compositions for etching other metallic material
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- ing And Chemical Polishing (AREA)
Abstract
The present disclosure provides a germanium ingot etching method, including the steps of: step one, cleaning germanium ingots by deionized water, and drying the germanium ingots by nitrogen; preparing concentrated acid corrosive liquid of nitric acid and hydrofluoric acid in a volume ratio of 2-3: 1, and preparing dilute acid corrosive liquid in a volume ratio of 2-3: 1: 4-6 of nitric acid, hydrofluoric acid and water; placing the concentrated acid corrosive liquid in a corrosion tank, placing the corrosion tank containing the concentrated acid in a pure water tank of a fume hood, setting the water bath temperature to be 18-25 ℃, and placing the corrosion tank containing the dilute acid on the fume hood; step four, heating the germanium ingot; putting the germanium ingot after temperature rise into concentrated acid to corrode for 1-3 min, and quickly putting the germanium ingot into a corrosion tank containing dilute acid to corrode for 1-2 min after the concentrated acid corrodes; putting the corroded germanium ingot into a pure water tank for repeated flushing, and drying by using nitrogen; step seven, placing the dried germanium ingots into a pp disc and covering the pp disc with a cover; the first step to the seventh step need to be operated in a hundred-grade clean room.
Description
Technical Field
The invention relates to the field of preparation of ultra-high purity germanium single crystals, in particular to a corrosion method of a germanium ingot.
Background
Before zone melting and single crystal pulling of high-purity germanium polycrystal, the raw material germanium ingot needs to be subjected to corrosion treatment. The existing corrosion method is not clean in corrosion, the surface of the germanium ingot is easily whitened and yellowed, cracks are easily generated in the corrosion of the germanium ingot, the cracks are not cleaned completely, impurities are accumulated at the cracks and are easily oxidized and whitened, the corrosion method is complicated, and alkali corrosion is needed after the acid corrosion is finished.
Disclosure of Invention
In view of the problems in the background art, it is an object of the present disclosure to provide etching of germanium ingots.
In order to achieve the above object, the present disclosure provides a method for etching a germanium ingot, comprising the steps of: step one, cleaning germanium ingots by using deionized water, and then drying by using nitrogen; preparing concentrated acid corrosive liquid of nitric acid and hydrofluoric acid in a volume ratio of 2-3: 1, and preparing dilute acid corrosive liquid in a volume ratio of 2-3: 1: 4-6 of nitric acid, hydrofluoric acid and water; placing the concentrated acid corrosive liquid in the step two in a corrosion tank, placing the corrosion tank containing the concentrated acid in a pure water tank of a fume hood, setting the water bath temperature to be 18-25 ℃, and placing the corrosion tank containing the dilute acid in the fume hood; step four, heating the germanium ingot in the step one; putting the germanium ingot after temperature rise into an etching tank containing concentrated acid for etching for 1-3 min, and quickly putting the germanium ingot into the etching tank containing dilute acid for etching for 1-2 min after the germanium ingot is etched by the concentrated acid; sixthly, putting the germanium ingots corroded in the fifth step into a pure water tank for repeated flushing, and drying by using nitrogen; step seven, placing the dried germanium ingots into a pp disc and covering the pp disc with a cover; the first step to the seventh step need to be operated in a hundred-grade clean room.
In some embodiments, in step one, the nitrogen is 9N of high purity nitrogen.
In some embodiments, in step two, the concentration of nitric acid is UP grade 65% -71%.
In some embodiments, in step four, the germanium ingot is warmed to 40 ℃ to 45 ℃.
In some embodiments, in step four, the germanium ingot is heated by putting the germanium ingot into pure water.
In some embodiments, in the fifth step, the germanium ingot after being heated is put into an etching tank containing concentrated acid to be etched for 1min to 2 min.
In some embodiments, in step five, after the concentrated acid etching, the germanium ingot is quickly put into an etching tank containing dilute acid to be etched for 1 min.
The beneficial effects of this disclosure are as follows:
the disclosure provides a method for corroding a germanium ingot, wherein the surface of the germanium ingot after corrosion is brighter and cleaner, the germanium ingot after corrosion does not turn white or yellow, and the germanium ingot after corrosion does not crack; the process provided by the present disclosure does not require a re-caustic etch after acid etching.
Detailed Description
The method of etching a germanium ingot according to the present disclosure is described in detail below.
The application discloses a germanium ingot corrosion method, which comprises the following steps: step one, cleaning germanium ingots by using deionized water, and then drying by using nitrogen; preparing concentrated acid corrosive liquid of nitric acid and hydrofluoric acid in a volume ratio of 2-3: 1, and preparing dilute acid corrosive liquid in a volume ratio of 2-3: 1: 4-6 of nitric acid, hydrofluoric acid and water; placing the concentrated acid corrosive liquid in the step two in a corrosion tank, placing the corrosion tank containing the concentrated acid in a pure water tank of a fume hood, setting the water bath temperature to be 18-25 ℃, and placing the corrosion tank containing the dilute acid on the fume hood; step four, heating the germanium ingot in the step one; putting the germanium ingot after temperature rise into an etching tank containing concentrated acid for etching for 1-3 min, and quickly putting the germanium ingot into the etching tank containing dilute acid for etching for 1-2 min after the germanium ingot is etched by the concentrated acid; sixthly, putting the germanium ingots corroded in the fifth step into a pure water tank for repeated flushing, and drying by using nitrogen; and step seven, putting the dried germanium ingots into a pp tray and covering the pp tray with a cover.
In some embodiments, steps one through seven need to be performed in a hundred-class clean room. Cleanliness is ensured at each step in the corrosion process, and no new impurities are introduced.
In some embodiments, in step one, the nitrogen is 9N of high purity nitrogen. In the first step, high-purity nitrogen is used and blown in a hundred-grade clean bench, and the purpose of blowing with high-purity nitrogen is to avoid introducing impurities or dust in the blowing process.
In the second step, the concentration of the nitric acid is 65-71% of UP grade in the second step.
And in the second step, the volume ratio of the concentrated acid etching solution is 2-3: 1. The surface of the corroded germanium ingot is brighter and cleaner, and the germanium ingot cannot turn white or yellow after being corroded. When the volume ratio of the nitric acid to the hydrofluoric acid is less than 2: 1, the concentration of the etching solution is high, the germanium ingot is excessively etched, and cracks are generated; when the volume ratio of the nitric acid to the hydrofluoric acid is more than 3: 1, the concentration of the nitric acid to the hydrofluoric acid is too low, the germanium ingot cannot be completely corroded, and impurities on the surface cannot be completely removed.
In the second step, the volume ratio of the dilute acid corrosive liquid is a mixed liquid of nitric acid, hydrofluoric acid and water which is 2-3: 1: 4-6. If the concentration of the dilute acid is too low, the concentration gradient of the concentrated dilute acid is too large, and germanium ingots can be hydrolyzed; if the concentration of the dilute acid is too high, no transition effect is realized, and the dilute acid can be hydrolyzed into pure water.
In the third step, the temperature of the water bath is set to be 18-25 ℃. Because the germanium ingots are severely corroded by the concentrated acid, the temperature is rapidly increased to about 70 ℃ from the normal temperature within 1min, the corrosion tank containing the concentrated acid is placed in a pure water tank at the temperature of 18-25 ℃ for water bath, the reaction is slowly carried out, the temperature is slowly increased, and the excessive violent reaction is avoided, so that the generation of cracks on the germanium ingots is avoided.
In some embodiments, in step four, the germanium ingot is heated by putting the germanium ingot into pure water.
In some embodiments, in step four, the germanium ingot is warmed to 40 ℃ to 45 ℃.
And in the fifth step, putting the germanium ingot after temperature rise into a corrosion tank filled with concentrated acid for corrosion, heating the germanium ingot and then starting corrosion, so as to avoid the phenomenon that the temperature difference between the inside of the germanium ingot and the surface is too large, so that the surface of the germanium ingot is rapidly contracted to generate cracks.
In the fifth step, the etching is firstly carried out in concentrated acid for 1min to 3min and then carried out in dilute acid for 1min to 2 min. The germanium ingots are prevented from being hydrolyzed directly from concentrated acid to pure water, and the concentration span is too large; and the phenomenon that the concentration of corrosive liquid on the surface of the germanium ingot is too high to contact with air and be oxidized in the process of directly taking the germanium ingot out of the concentrated acid is also avoided.
In some embodiments, in step five, after the concentrated acid etching, the germanium ingot is quickly put into an etching tank containing dilute acid to be etched for 1 min.
The method provided by the present disclosure does not require any further alkaline etching.
[ test procedures and test results ].
Example 1
The following operations are all performed in a hundred-grade clean room or with cleanliness higher than hundred-grade:
step one, cleaning germanium ingots by using deionized water, and then drying by using nitrogen;
preparing concentrated acid corrosive liquid of nitric acid and hydrofluoric acid in a volume ratio of 2: 1, and preparing dilute acid corrosive liquid in a volume ratio of nitric acid, hydrofluoric acid and water of 3: 1: 5;
placing the concentrated acid corrosive liquid in the step two in a corrosion tank, placing the corrosion tank containing the concentrated acid in a pure water tank of a fume hood, setting the water bath temperature to be 20 ℃, and placing the corrosion tank containing the dilute acid in the fume hood;
step four, boiling and heating the germanium ingots obtained in the step one to 40-45 ℃;
putting the germanium ingot after temperature rise into an etching tank containing concentrated acid for etching for 2min, and quickly putting the germanium ingot into the etching tank containing dilute acid for etching for 1min after the germanium ingot is etched by the concentrated acid;
sixthly, putting the germanium ingots corroded in the fifth step into a pure water tank for repeated flushing, and drying by using nitrogen;
and step seven, placing the dried germanium ingots into a pp tray and covering the pp tray with a cover.
Comparative example 1:
corroding germanium ingots according to the method in the embodiment 1, except that pure water is slowly added into a corrosion tank for dilution after the germanium ingots are corroded by concentrated acid for 2 minutes until red smoke turns yellow smoke, reacting for one minute, adding pure water into the corrosion tank again, taking out the germanium ingots for washing after the germanium ingots are not obviously corroded, and because the quantity of corroded germanium ingots is large, the required acid quantity is large, adding pure water into the concentrated acid corrosion tank for dilution, the acid in each corrosion tank can only be used once, the acid is wasted, a large amount of waste acid is generated, and the cost is increased; because the concentrated acid corrodes the tank and reacts violently, when pure water is added for dilution, acid is easy to splash, and potential safety hazards exist.
Comparative example 2:
germanium ingots were etched as in example 1, except that the process was operated in an environment with less than one hundred degrees of cleanliness, resulting in particulate dust from the environment adhering to the surface of the germanium ingot.
Comparative example 3:
germanium ingots were etched as in example 1, except that the germanium ingots were not cleaned prior to etching, and were directly etched, resulting in particulate dust from the germanium ingots adhering to the surface of the germanium ingots entering the germanium ingot pores during etching.
Comparative example 4:
and corroding germanium ingots according to the method in the embodiment 1, except that the corrosion time in concentrated acid is too long, after 2-3 min of corrosion, the temperature is continuously increased, the corrosion is too severe, the corrosion liquid is boiled violently, the germanium ingots move and contact with each other, so that the corrosion of the contact part is insufficient, and the contact part is blackened.
Comparative example 5:
the germanium ingot was etched according to the method of example 1, except that the concentrated acid etching solution was nitric acid and hydrofluoric acid at a ratio of 4: 1, which resulted in poor etching effect of the germanium ingot and failed to completely etch impurities embedded in the surface of the germanium ingot.
Comparative example 6:
germanium ingots were etched as in example 1, except that the concentrated acid etching solution was 1: 1 nitric acid to hydrofluoric acid, which was too aggressive and uncontrollable and easily oxidized during the transition from concentrated acid to dilute acid.
Comparative example 7:
the germanium ingot is corroded according to the method in the embodiment 1, except that the temperature of the germanium ingot is not raised to 40-45 ℃ before corrosion, when the germanium ingot is corroded by concentrated acid, the surface temperature of the germanium ingot can be rapidly raised to 70 ℃ from 25 ℃ of the room temperature, and cracks are easily generated due to the fact that the temperature difference between the inside and the outside of the germanium ingot is too large.
Comparative example 8:
germanium ingots were etched as in example 1, except that the concentrated acid etch bath was not placed in pure water at 20 ℃ for direct etching, the reaction was too vigorous and uncontrollable, and the germanium ingot surface was prone to blackening.
Comparative example 9:
germanium ingots were etched as in example 1 except that with the dilute acid etch removed, the germanium ingots were directly from concentrated acid to pure water and the concentration gradient was too great and hydrolysis of the germanium ingots occurred.
Comparative example 10:
the germanium ingot was etched according to the method of example 1, except that concentrated nitric acid and hydrofluoric acid were changed from 2: 1 to 2: 1, and hydrogen peroxide and hydrofluoric acid were changed from 2: 1, resulting in poor etching effect and poor removal of impurities on the surface of the germanium ingot.
Comparative example 11:
the germanium ingot was etched according to the method of example 1, except that concentrated nitric acid and hydrofluoric acid were changed from 2: 1 to 2: 1, hydrogen peroxide and hydrochloric acid were changed from 2: 1, resulting in poor etching effect and poor removal of impurities on the surface of the germanium ingot.
Comparative example 12:
germanium ingots were etched as in example 1 except that nitrogen gas having a purity of less than 9N was used for blow-drying, and particulate dust in the gas adhered to the surface of the germanium ingots, causing contamination.
Comparative example 13:
the germanium ingot is corroded according to the method in the embodiment 1, except that the cleaned germanium ingot is not soaked by pure water and is directly placed in a pure water tank to be dried, and micron-sized particle dust in a clean room falls on the surface of the germanium ingot to cause pollution in the process of being dried.
Comparative example 14:
germanium ingots were etched as in example 1 except that the dried germanium ingots were not covered with a lid and micron-sized particle dust in the clean room dropped on the surface of the germanium ingots, causing contamination.
The above-disclosed features are not intended to limit the scope of practice of the present disclosure, and therefore, all equivalent variations that are described in the claims of the present disclosure are intended to be included within the scope of the claims of the present disclosure.
Claims (7)
1. A method for etching a germanium ingot, comprising the steps of:
step one, cleaning germanium ingots by using deionized water, and then drying by using nitrogen;
preparing concentrated acid corrosive liquid of nitric acid and hydrofluoric acid in a volume ratio of 2-3: 1, and preparing dilute acid corrosive liquid in a volume ratio of 2-3: 1: 4-6 of nitric acid, hydrofluoric acid and water;
placing the concentrated acid corrosive liquid in the step two in a corrosion tank, placing the corrosion tank containing the concentrated acid in a pure water tank of a fume hood, setting the water bath temperature to be 18-25 ℃, and placing the corrosion tank containing the dilute acid on the fume hood;
step four, heating the germanium ingot in the step one;
putting the germanium ingot after temperature rise into an etching tank containing concentrated acid for etching for 1-3 min, and quickly putting the germanium ingot into the etching tank containing dilute acid for etching for 1-2 min after the germanium ingot is etched by the concentrated acid;
sixthly, putting the germanium ingots corroded in the fifth step into a pure water tank for repeated flushing, and drying by using nitrogen;
step seven, placing the dried germanium ingots into a pp disc and covering the pp disc with a cover;
the first step to the seventh step need to be operated in a hundred-grade clean room.
2. The method of etching a germanium ingot according to claim 1,
in step one, the nitrogen gas is 9N of high purity nitrogen gas.
3. The method of etching a germanium ingot according to claim 1,
in the second step, the concentration of the nitric acid is 65-71% of UP grade.
4. The method of etching a germanium ingot according to claim 1,
in the fourth step, the germanium ingot is heated to 40-45 ℃.
5. The method of etching a germanium ingot according to claim 1,
in the fourth step, the germanium ingot heating method is to put the germanium ingot into pure water for heating.
6. The method of etching a germanium ingot according to claim 1,
and in the fifth step, putting the germanium ingots after being heated into a corrosion tank containing concentrated acid to be corroded for 1-2 min.
7. The method of etching a germanium ingot according to claim 1,
in the fifth step, after the corrosion of the concentrated acid, the germanium ingot is quickly put into a corrosion tank containing the dilute acid to be corroded for 1 min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114250371A (en) * | 2021-12-27 | 2022-03-29 | 广东先导微电子科技有限公司 | Preparation method of high-purity antimony rod |
| CN115386962A (en) * | 2022-08-22 | 2022-11-25 | 中锗科技有限公司 | High-strength high-toughness ultrathin germanium single crystal wafer corrosion method |
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| CN115386962B (en) * | 2022-08-22 | 2023-12-22 | 中锗科技有限公司 | High-strength high-toughness ultrathin germanium single-crystal corrosion method |
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