CN110453289A - A kind of corrosive liquid and caustic solution for the identification of surface of indium phosphide twin - Google Patents
A kind of corrosive liquid and caustic solution for the identification of surface of indium phosphide twin Download PDFInfo
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- CN110453289A CN110453289A CN201910885871.9A CN201910885871A CN110453289A CN 110453289 A CN110453289 A CN 110453289A CN 201910885871 A CN201910885871 A CN 201910885871A CN 110453289 A CN110453289 A CN 110453289A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B33/00—After-treatment of single crystals or homogeneous polycrystalline material with defined structure
- C30B33/08—Etching
- C30B33/10—Etching in solutions or melts
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
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Abstract
The present invention relates to a kind of corrosive liquids and caustic solution for the identification of surface of indium phosphide twin, belong to field of semiconductor materials.The present invention is used for the corrosive liquid of surface of indium phosphide twin identification, the component comprising following percent by volume: hydrochloric acid 30%~70%, hydrogen peroxide 0%~35%, acetic acid 20%~70%.The present invention is used for the caustic solution of surface of indium phosphide twin identification, comprising the following steps: (1) impregnates inp wafer with alcohol；(2) inp wafer surface is rinsed with deionized water；(3) inp wafer is put into corrosive liquid and is impregnated；(4) inp wafer surface, and dry inp wafer are rinsed with deionized water；(5) inp wafer surface is observed under fluorescent light and marks twin distribution.Identify that stability is high, reproducible, corrosion rate is controllable for surface of indium phosphide twin using corrosive liquid and caustic solution of the invention.
Description
Technical field
The present invention relates to a kind of corrosive liquids and caustic solution for the identification of surface of indium phosphide twin, belong to semiconductor material
Field.
Background technique
As a kind of important III -- V group iii v compound semiconductor material, indium phosphide (InP) have many excellent performances,
Such as: direct transition type band structure, forbidden bandwidth is wider, photoelectric conversion efficiency is higher, electron mobility is high, capability of resistance to radiation compared with
It is strong etc..Therefore, indium phosphide is widely used in the fields such as high-frequency microwave device and circuit, solar battery, fiber optic communication.
Currently, being proposed to material higher with using indium phosphide as the development of the devices such as the microelectronics of substrate and photoelectron
Requirement, it is whether most important to indium phosphide extension containing twin in indium phosphide single crystal.Since the stacking fault energy of indium phosphide exists
It is minimum in several semiconductor materials, therefore easily occur twin in the production process of indium phosphide single crystal.Although reducing the production of twin
Life is the emphasis of indium phosphide single crystal growing technology, but still cannot avoid the generation of twin completely, and tiny twin is not easy to know
Not.Therefore, indium phosphide finds that there is twin on surface, will cause the loss of chip and the waste of manpower and material resources after polished and cleaned.
Indium phosphide can react at room temperature with hydrochloric acid, and for (100) indium phosphide, hydrochloric acid is a kind of very effective
Corrosive agent, anisotropic etching characteristic is clearly.But since corrosion rate of the indium phosphide in hydrochloric acid is too fast, it is difficult to control
System, therefore cannot be used for the identification of chip twin.
Zheng Jianhe discusses different corrosive liquids to changing after InP burnishing surface photoetching in document " chemical attack of InP "
The effect for learning corrosion, analyzes effect of the different corrosive liquids to InP, has studied etching time, the corrosion speed of different corrosive liquids
Degree and corrosion angle are to the section figure of different crystal orientations chip and the influence of wafer surface.
Xu Zhaopeng is begged in document " chemical attack of GaAs, GaP, InP, InGaAsP, AlGaAs, InAlGaAs are studied "
Discussed chemical attack itself by aoxidize -- based on complex Theory, corrosive agent generally include oxidation, complexing dissolution, dilution three kinds at
Part, the oxide that corrosion process is oxidized agent oxidation comprising wafer surface layer and generates is dissolved by complexing；For different substrates
Material has carried out chemical attack experimental study, for grinding for the devices chemical attacks such as optoelectronic intagration photoswitch and micro-slice laser
System provides direction.
Summary of the invention
It is provided a kind of twin for surface of indium phosphide it is an object of the invention to overcome above-mentioned the deficiencies in the prior art place
The corrosive liquid and caustic solution of crystalline substance identification carry out chemical attack using corrosive liquid of the invention, and stability is high, reproducible, rotten
It is controllable to lose speed.
To achieve the above object, the technical scheme adopted by the invention is as follows: it is a kind of for surface of indium phosphide twin identification corruption
Lose liquid, the component comprising following percent by volume: hydrochloric acid 30%~70%, hydrogen peroxide 0%~35%, acetic acid 20%~70%.
As the preferred embodiment of corrosive liquid of the present invention, the component comprising following percent by volume: hydrochloric acid 40%
~60%, hydrogen peroxide 0%~10%, acetic acid 30%~60%.
As the preferred embodiment of corrosive liquid of the present invention, the component comprising following percent by volume: hydrochloric acid 60%,
Hydrogen peroxide 10%, acetic acid 30%.
As the preferred embodiment of corrosive liquid of the present invention, the hydrochloric acid is the salt of mass fraction 36%~38%
Acid, the hydrogen peroxide are the hydrogen peroxide of mass fraction 30%~32%, and the acetic acid is the vinegar of mass fraction 99.7%~100%
Acid.
The present invention also provides a kind of caustic solutions for the identification of surface of indium phosphide twin, and the caustic solution is using above-mentioned
Corrosive liquid.
Preferred embodiment as caustic solution of the present invention, comprising the following steps:
(1) inp wafer is impregnated with alcohol；
(2) inp wafer surface then is rinsed with deionized water；
(3) inp wafer after rinsing step (2), which is put into corrosive liquid, to be impregnated；
(4) inp wafer surface, and dry inp wafer then are rinsed with deionized water；
(5) inp wafer surface is observed under fluorescent light and marks twin distribution.
As the preferred embodiment of caustic solution of the present invention, in the step (1), the mass fraction of alcohol is
80%~98%, soaking time is 20~30min, and soaking temperature is 10~40 DEG C.
As the preferred embodiment of caustic solution of the present invention, in the step (2), floated using deionized water overflow
The mode washed or arrange bath fastly or a combination of both rinses inp wafer surface, rinses 30~120s, then manual flush 30s.
As the preferred embodiment of caustic solution of the present invention, in the step (3), soaking temperature is 10~40
DEG C, soaking time is 30~180s, inp wafer uniform stroke in corrosive liquid in soaking process.
As the preferred embodiment of caustic solution of the present invention, in the step (4), floated using deionized water overflow
The mode washed or arrange bath fastly or a combination of both rinses inp wafer surface, rinses 30~90s, then manual flush 20~
60s；Then inp wafer being impregnated in alcohol with the dry chip of hot nitrogen after 2~10s, drying temperature is 40~50 DEG C,
Drying time is 30~90s.
As the preferred embodiment of caustic solution of the present invention, in the step (5), from inp wafer front and back sides
Different angle observation twin distributions.
Compared with prior art, the invention has the benefit that being used for phosphorus using corrosive liquid and caustic solution of the invention
Change the identification of indium surface twin, stability is high, reproducible, corrosion rate is controllable.The present invention compares hcl corrosion, and controllability is more
By force；When using hcl corrosion, the amount of eroding is 30~50 μm/min；The rate of dissolution of indium phosphide is slow in corrosion process of the present invention,
The amount of eroding is 3~15 μm/min；After corrosion, the distribution of surface of indium phosphide twin is readily identified, so that processing efficiency is improved,
Save cost.
Detailed description of the invention
Fig. 1 is flow chart of the present invention for the caustic solution of surface of indium phosphide twin identification.
Specific embodiment
Purposes, technical schemes and advantages in order to better illustrate the present invention, below in conjunction with the drawings and specific embodiments pair
The present invention is described further.
Embodiment 1
Flow chart of the present embodiment for the caustic solution of surface of indium phosphide twin identification is as shown in Figure 1.
5 with a thickness of 450~460 μm of 4 cun of indium phosphide (InP) chips it is sliced after be put into wafer case (Cassette)
In, it is to impregnate 20min at 10 DEG C in 80% alcohol that the Cassette equipped with chip, which is placed in mass fraction,；Chip will be housed
Cassette is placed in overflow launder, rinses 30s with the mode that fast row's bath combines with deionized water overflow rinsing, then be subject to
Manual flush 30s；It is hydrochloric acid 30%, acetic acid 50%, hydrogen peroxide that the Cassette equipped with chip, which is immersed volume ratio, later
In 20% solution, wherein hydrochloric acid is the hydrochloric acid of mass fraction 36%~38%, and hydrogen peroxide is mass fraction 30%~32%
Hydrogen peroxide, acetic acid are the acetic acid of mass fraction 99.7%~100%, at the uniform velocity shake 180s at 10 DEG C of corrosive liquid temperature；Then
The Cassette equipped with chip is placed in overflow launder immediately, the side combined with deionized water overflow rinsing with fast row's bath
Formula rinses 30s, then is subject to manual flush 20s；It being put into alcohol and impregnates 2s, then dried up with hot nitrogen, drying temperature is 40 DEG C,
Drying time is 30s.Under fluorescent light, observe wafer surface twin distribution, from the different angle in chip front and back sides (0~
180 °) observation twin distribution, and identify twin position.
Test result: observe that the main back side of chip is smooth and uniformity, brightness are normal after corrosion under fluorescent light；Chip
The amount of eroding is 14 μm/min, can clearly identify that wafer surface twin is distributed.
Embodiment 2
5 with a thickness of 460~470 μm of 4 cun of indium phosphide (InP) chips it is sliced after be put into wafer case (Cassette),
It is to impregnate 30min at 40 DEG C in 98% alcohol that Cassette equipped with chip, which is placed in mass fraction,；Chip will be housed
Cassette is placed in overflow launder, rinses 120s with the fast row mode combined of washing by water with deionized water overflow rinsing, then plus
With manual flush 30s；It is hydrochloric acid 70%, acetic acid 20%, hydrogen peroxide that the Cassette equipped with chip, which is immersed volume ratio, later
In 10% solution, wherein hydrochloric acid is the hydrochloric acid of mass fraction 36%~38%, and hydrogen peroxide is mass fraction 30%~32%
Hydrogen peroxide, acetic acid are the acetic acid of mass fraction 99.7%~100%, at the uniform velocity shake 30s at 40 DEG C of corrosive liquid temperature；Then it stands
It will be placed in overflow launder equipped with the Cassette of chip, the mode combined with deionized water overflow rinsing with fast row's bath
90s is rinsed, then is subject to manual flush 60s；It being put into alcohol and impregnates 10s, then dried up with hot nitrogen, drying temperature is 50 DEG C,
Drying time is 90s.Under fluorescent light, observe wafer surface twin distribution, from the different angle in chip front and back sides (0~
180 °) observation twin distribution, and identify twin position.
Test result: observe that the main back side of chip is smooth and uniformity, brightness are normal after corrosion under fluorescent light；Chip
The amount of eroding is 11 μm/min, can clearly identify that wafer surface twin is distributed.
Embodiment 3
5 with a thickness of 440~450 μm of 4 cun of indium phosphide (InP) chips it is sliced after be put into wafer case (Cassette),
It is to impregnate 30min at 20 DEG C in 98% alcohol that Cassette equipped with chip, which is placed in mass fraction,；Chip will be housed
Cassette is placed in overflow launder, rinses 70s with the mode that fast row's bath combines with deionized water overflow rinsing, then be subject to
Manual flush 30s；The Cassette equipped with chip is immersed in the solution that volume ratio is hydrochloric acid 30%, acetic acid 70% later,
Wherein, hydrochloric acid is the hydrochloric acid of mass fraction 36%~38%, and acetic acid is the acetic acid of mass fraction 99.7%~100%, is being corroded
90s is at the uniform velocity shaken at 20 DEG C of liquid temperature；The Cassette equipped with chip is placed in overflow launder immediately after, uses deionized water
Overflow rinsing rinses 80s with the mode that fast row's bath combines, then is subject to manual flush 30s；It is put into alcohol and impregnates 4s, then
It is dried up with hot nitrogen, drying temperature is 45 DEG C, drying time 70s.Under fluorescent light, the twin distribution of wafer surface is observed,
Twin is distributed from the different angle in chip front and back sides (0~180 °), and identifies twin position.
Test result: observe that the main back side of chip is smooth and uniformity, brightness are normal after corrosion under fluorescent light；Chip
The amount of eroding is 11 μm/min, can clearly identify that wafer surface twin is distributed.
Embodiment 4
5 with a thickness of 440~450 μm of 4 cun of indium phosphide (InP) chips it is sliced after be put into wafer case (Cassette),
It is to impregnate 30min at 20 DEG C in 98% alcohol that Cassette equipped with chip, which is placed in mass fraction,；Chip will be housed
Cassette is placed in overflow launder, rinses 70s with the mode that fast row's bath combines with deionized water overflow rinsing, then be subject to
Manual flush 30s；It is hydrochloric acid 60%, acetic acid 30%, hydrogen peroxide that the Cassette equipped with chip, which is immersed volume ratio, later
In 10% solution, wherein hydrochloric acid is the hydrochloric acid of mass fraction 36%~38%, and hydrogen peroxide is mass fraction 30%~32%
Hydrogen peroxide, acetic acid are the acetic acid of mass fraction 99.7%~100%, at the uniform velocity shake 50s at 20 DEG C of corrosive liquid temperature；Then it stands
It will be placed in overflow launder equipped with the Cassette of chip, the mode combined with deionized water overflow rinsing with fast row's bath
60s is rinsed, then is subject to manual flush 30s；It is put into alcohol and impregnates 4s, then dried up with hot nitrogen, drying temperature is 45 DEG C, is done
The dry time is 70s.Under fluorescent light, the twin distribution for observing wafer surface, from the different angle in chip front and back sides (0~180 °)
Twin distribution is observed, and identifies twin position.
Test result: observe that the main back side of chip is smooth and uniformity, brightness are normal after corrosion under fluorescent light；Chip
The amount of eroding is 12 μm/min, can clearly identify that wafer surface twin is distributed.
Comparative example 1
5 with a thickness of 440~450 μm of 4 cun of indium phosphide (InP) chips it is sliced after be put into wafer case (Cassette),
It is to impregnate 30min at 20 DEG C in 98% alcohol that Cassette equipped with chip, which is placed in mass fraction,；Chip will be housed
Cassette is placed in overflow launder, rinses 70s with the mode that fast row's bath combines with deionized water overflow rinsing, then be subject to
Manual flush 30s；The Cassette equipped with chip is immersed in the hydrochloric acid that mass fraction is 36%~38% later, in corrosive liquid
50s is at the uniform velocity shaken at 20 DEG C of temperature；The Cassette equipped with chip is placed in overflow launder immediately after, is overflow with deionized water
Stream rinsing rinses 60s with the mode that fast row's bath combines, then is subject to manual flush 30s；It is put into alcohol and impregnates 4s, then use
Hot nitrogen drying, drying temperature are 45 DEG C, drying time 70s.Under fluorescent light, the twin distribution for observing wafer surface, from
(0~180 °) the observation twin distribution of the different angle in chip front and back sides, and identify twin position.
Test result: observe that the main back side of chip is smooth and uniformity, brightness are normal after corrosion under fluorescent light；Chip
The amount of eroding is 45 μm/min, can clearly identify that wafer surface twin is distributed.
Effect example 1
The proportion of corrosive liquid each component of the present invention influences the effect of surface of indium phosphide twin identification, to investigate each group distribution ratio
Test group 1~8 and control group 1~3 is arranged in influence to surface of indium phosphide twin recognition effect.Test group 1~8 and control group 1
In~3, only hydrochloric acid, hydrogen peroxide, the percent by volume of acetic acid are different in corrosive liquid, and are selected respectively according to the different ratio of corrosive liquid
More preferred etching time is taken, remaining etching condition is the same as embodiment 1.Corrosive liquid each group in test group 1~8 and control group 1~3
Point percent by volume it is as shown in table 1, and in accordance with the above-mentioned embodiment 1~4 in test method tested, test result such as table
Shown in 1.
Table 1
As shown in Table 1, the proportion of corrosive liquid each component of the present invention influences the effect of surface of indium phosphide twin identification, works as each group
Distribution ratio within the scope of the present invention when, corroded using corrosive liquid of the invention, have the lower amount of eroding, indium phosphide table
Twin distribution in face readily identifies；When hydrochloric acid in corrosive liquid percent by volume be 40%~60%, the volume basis of hydrogen peroxide
Than being 0%~10%, when the percent by volume of acetic acid is 30%~60%, is corroded using corrosive liquid of the invention, had
The lower amount of eroding, the distribution of surface of indium phosphide twin readily identify；When hydrochloric acid in corrosive liquid percent by volume be 60%,
The percent by volume of hydrogen peroxide is 10%, when the percent by volume of acetic acid is 30%, is corroded using corrosive liquid of the invention,
With the minimum amount of eroding, the distribution of surface of indium phosphide twin is readily identified.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention rather than protects to the present invention
The limitation of range is protected, although the invention is described in detail with reference to the preferred embodiments, those skilled in the art should
Understand, it can be with modification or equivalent replacement of the technical solution of the present invention are made, without departing from the essence of technical solution of the present invention
And range.
Claims (10)
1. a kind of corrosive liquid for the identification of surface of indium phosphide twin, which is characterized in that the component comprising following percent by volume:
Hydrochloric acid 30%~70%, hydrogen peroxide 0%~35%, acetic acid 20%~70%.
2. corrosive liquid as described in claim 1, which is characterized in that the component comprising following percent by volume: hydrochloric acid 40%~
60%, hydrogen peroxide 0%~10%, acetic acid 30%~60%.
3. corrosive liquid as claimed in claim 2, which is characterized in that the component comprising following percent by volume: hydrochloric acid 60%, double
Oxygen water 10%, acetic acid 30%.
4. corrosive liquid as described in claim 1, which is characterized in that the hydrochloric acid is the hydrochloric acid of mass fraction 36%~38%,
The hydrogen peroxide is the hydrogen peroxide of mass fraction 30%~32%, and the acetic acid is the acetic acid of mass fraction 99.7%~100%.
5. a kind of caustic solution for the identification of surface of indium phosphide twin, which is characterized in that the caustic solution is wanted using right
Seek 1~4 described in any item corrosive liquids.
6. caustic solution as claimed in claim 5, which comprises the following steps:
(1) inp wafer is impregnated with alcohol；
(2) inp wafer surface then is rinsed with deionized water；
(3) inp wafer after rinsing step (2), which is put into corrosive liquid, to be impregnated；
(4) inp wafer surface, and dry inp wafer then are rinsed with deionized water；
(5) inp wafer surface is observed under fluorescent light and marks twin distribution.
7. caustic solution as claimed in claim 6, which is characterized in that in the step (1), the mass fraction of alcohol is 80%
~98%, soaking time is 20~30min, and soaking temperature is 10~40 DEG C.
8. caustic solution as claimed in claim 6, which is characterized in that in the step (2), rinsed using deionized water overflow
Or the mode of fast row's bath or a combination of both rinses inp wafer surface, rinses 30~120s, then manual flush 30s.
9. caustic solution as claimed in claim 6, which is characterized in that in the step (3), soaking temperature is 10~40 DEG C,
Soaking time is 30~180s, inp wafer uniform stroke in corrosive liquid in soaking process.
10. caustic solution as claimed in claim 6, which is characterized in that in the step (4), floated using deionized water overflow
The mode washed or arrange bath fastly or a combination of both rinses inp wafer surface, rinses 30~90s, then manual flush 20~
60s；Then inp wafer being impregnated in alcohol with the dry chip of hot nitrogen after 2~10s, drying temperature is 40~50 DEG C,
Drying time is 30~90s；In the step (5), twin is distributed from the angle different from inp wafer front and back sides.
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| CN113427651A (en) * | 2021-06-25 | 2021-09-24 | 广东先导微电子科技有限公司 | Method for judging linear twin crystal length in gallium arsenide crystal |
| CN114540033A (en) * | 2022-01-13 | 2022-05-27 | 北京通美晶体技术股份有限公司 | Indium phosphide thinning corrosion solution and application thereof |
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| CN113427651A (en) * | 2021-06-25 | 2021-09-24 | 广东先导微电子科技有限公司 | Method for judging linear twin crystal length in gallium arsenide crystal |
| CN114540033A (en) * | 2022-01-13 | 2022-05-27 | 北京通美晶体技术股份有限公司 | Indium phosphide thinning corrosion solution and application thereof |
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