CN104241116B - A kind of method of germanium material surface-stable passivation - Google Patents
A kind of method of germanium material surface-stable passivation Download PDFInfo
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- CN104241116B CN104241116B CN201410404017.3A CN201410404017A CN104241116B CN 104241116 B CN104241116 B CN 104241116B CN 201410404017 A CN201410404017 A CN 201410404017A CN 104241116 B CN104241116 B CN 104241116B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02041—Cleaning
- H01L21/02043—Cleaning before device manufacture, i.e. Begin-Of-Line process
- H01L21/02052—Wet cleaning only
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02225—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer
- H01L21/02227—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a process other than a deposition process
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02225—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer
- H01L21/02227—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a process other than a deposition process
- H01L21/0223—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a process other than a deposition process formation by oxidation, e.g. oxidation of the substrate
- H01L21/02233—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a process other than a deposition process formation by oxidation, e.g. oxidation of the substrate of the semiconductor substrate or a semiconductor layer
- H01L21/02236—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a process other than a deposition process formation by oxidation, e.g. oxidation of the substrate of the semiconductor substrate or a semiconductor layer group IV semiconductor
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Abstract
The present invention relates to a kind of method of germanium material surface-stable passivation, including：Germanium wafer surface is cleaned using different reagents, germanium surface contaminants and superficial oxidation layer is effectively removed, realizes the first one-step chlorination on germanium surface；Then the Compound mixed solution thiol reagent of second alcohol and water is used, self-assembled film is obtained on germanium surface using the passivating conditions suitably heated.The present invention has the advantages that simple to operate, easy to use, with low cost, passivation effect is obvious.
Description
Technical field
The invention belongs to germanium material field of surface treatment, more particularly to a kind of method of germanium material surface-stable passivation.
Background technology
The electronic device of current semi-conducting material makes it in bio-sensing application because of its high sensitivity and excellent selectivity
In be developed rapidly.As a kind of typical semi-conducting material, the biology sensor based on silicon materials has been widely studied.
And it is used as the semi-conducting material of the same clan of silicon --- germanium (Ge), compared with Si, Ge electronics and hole mobility are 3 times of Si respectively
With 4 times, and Ge energy gap is more much smaller than Si.Therefore, Ge can realize the electronics device of high mobility as channel material
Part, is expected to be used widely in high-performance biochemical sensor field.But it is used as a kind of semiconductor material found prior to Si
Material, Ge can form stable surface oxide layer (SiO unlike Si2), easy generation dielectric under Ge material surface natures
Oxide layer (the GeO that constant is small, heat endurance is poor and defect concentration is bigx), and oxide layer composition by humidity, crystal orientation, illumination
Deng the influence of many factors.Although Ge is used for the preparation of semiconductor devices prior to Si, it is a lack of stable surface and greatly presses down
Fast development of the Ge materials in microelectronic has been made, and then have impact on its application in biological electronics field.
Want Ge materials being used for biochemical sensitive field, be the Ge materials for needing to obtain surface-stable the problem of primary.
(G.Collins, J.D.Holmes.Chemical in a series of Ge surface passivation methods reported at present
functionalisation of silicon and germanium nanowires[J].Journal of Materials
Chemistry,2011,21(30):11052-11069), Ge tables first typically are removed with halogen acids (HF, HCl, HBr and HI etc.)
The oxide layer in face, realizes the preliminary passivation on Ge surfaces, then by with Grignard reagents, photochemistry, diazol or germane
Change the effect that reaction reaches surface passivation.From the point of view of the result reported at present, in a variety of Ge surface passivation treatment methods, pass through
The Ge surfaces of HF processing can only maintain stability (T.Deegan, the G.Hughes.An X-ray of more than ten minutes in atmosphere
photoelectron spectroscopy study of the HF etching of native oxides on Ge
(111)and Ge(100)surfaces[J].Applied Surface Science,1998,123:66-70), HCl is passed through
The Ge surface stabilities of processing also no more than 2h (D.Bodlaki, H.Yamamoto, D.H.Waldeck,
E.Borguet.Ambient stability of chemically passivated germanium interfaces[J]
.Surface Science,2003,543:63-74；CN103681245A).In addition, the length realized by Ge-C or Ge-S connections
Carbochain (- (CH2)n-) protection energy duration is typically also no more than 48h (CN102005390B), and the stabilization time is such as
Fruit can substantially reduce under the conditions of aqueous phase (high humility), and these are all unfavorable for the subsequent applications of Ge materials.Therefore, it is badly in need of one at present
Efficient Ge surface passivation methods are planted, the long-time passivation protection of Ge material surfaces can be realized.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of method of germanium material surface-stable passivation, and this method passes through
The composition of reaction system and the temperature of reaction are adjusted, effective removal of Ge surface oxide layers is realized, while Ge surfaces can be realized
Overstable passivation protection.
A kind of method of germanium material surface-stable passivation of the present invention, including：
(1) Ge pieces are sequentially placed into acetone and ethanol solution and be cleaned by ultrasonic, effectively remove the organic of Ge pieces surface
Pollutant；
(2) soaking and washing is carried out to Ge pieces using deionized water and hydrochloric acid solution successively, effectively removes Ge piece remained on surface
Oxide layer and metal ion；
(3) it is formulated for the thiol solution of passivation；
Passivation Treatment in thiol solution will be dipped at (4) 60~80 DEG C with cleaned Ge pieces, you can so that Ge surfaces
Thiol molecule in self assembly, obtains overstable this surface of passivation.
Ge pieces in the step (1) are the Ge pieces of crystal orientation (100), (110) or (111), or to be grown on insulating barrier
Ge.
Hydrochloric acid is formed by mass percent for 38.3% analysis pure hydrochloric acid deionized water dilution in the step (2),
Mass percent is 5~10%.
The processing time of deionized water and hydrochloric acid is 30min~2h in the step (2).
Thiol solution concentration is 0.1~10mmol/L in the step (3), and solvent for use is the mixed liquor of second alcohol and water,
The percent by volume of its reclaimed water is 10~50%.
The mercaptan is CH3(CH2)nSH typically contains Long carbon chain, and n >=9 are typical such as lauryl mercaptan, 16 mercaptan, ten
Eight mercaptan etc..
The Passivation Treatment time is 12~24h in the step (4), and passivation reaction system needs to seal to reduce waving for ethanol
Hair.Other processing are completed under room temperature (25 DEG C or so).
Beneficial effect
(1) present invention effectively removes Ge surface contaminants and superficial oxidation layer, and realize the preliminary chlorine on Ge surfaces
Change (Ge-Cl), the Ge surfaces of cleaning are provided for follow-up passivation；
(2) present invention uses the Compound mixed solution thiol reagent of second alcohol and water, and one side ethanol can effectively disperse to be insoluble in
The thiol reagent of water, the water on the other hand dissolved each other with ethanol can effectively suppress extraneous residual oxygen to self assembly in passivating process
Passivating film oxidative attack；
(3) on the one hand the present invention can effectively accelerate the formation speed of self assembly passivating film using the passivating conditions suitably heated
Degree, on the other hand can improve the compactness and stability of self-assembled film；
(4) the passivation Ge for preparing of the present invention under atmospheric environment can for a long time (>15 days) remain stable, it is far longer than and has reported
The 48h in road, its stabilization time under the conditions of aqueous phase (high humility) also above 10 days, much larger than a few hours reported for work；
(5) the Ge surface cleans that provide of the present invention and the method for passivation, with it is simple to operate, easy to use, with low cost,
The advantages of passivation effect is obvious.
Brief description of the drawings
Fig. 1 for the present invention provide it is this Ge pieces are cleaned and surface passivation principle schematic；Wherein, (a) is passed through
Cross the blank Ge prints that acetone is cleaned with ethanol；(b) after deionized water and HCl treatment surface chlorination Ge prints；(c)
The Ge prints being passivated using mercaptan (R-SH)；1 is germanium oxide (GeOx, including+1, a variety of valence states such as+2 ,+3 ,+4)；2 be germanium material
Expect (zero-valent state)；3 be the germanium material surface of surface chlorination；4 be thiol molecule (R-SH；
Fig. 2 be the embodiment of the present invention Ge pieces are cleaned and surface passivation schematic flow sheet；
Fig. 3 is x-ray photoelectron power spectrum (XPS) result of the embodiment of the present invention through Ge prints Ge3d before HCl treatment；
Fig. 4 ties for Ge prints Ge3d and Cl2p after HCl treatment of embodiment of the present invention x-ray photoelectron power spectrum (XPS)
Really, it is specially：(a) it is x-ray photoelectron power spectrum (XPS) result of Ge prints Ge3d after HCl treatment；(b) for after HCl treatment
Ge prints Cl2p x-ray photoelectron power spectrum (XPS) result；
Fig. 5 is C1s of the embodiment of the present invention through n- dodecyl mereaptan (NDM) Passivation Treatment Ge x-ray photoelectron power spectrum
(XPS) Comparative result result；
Fig. 6 is water contact angle stability comparing result of the embodiment of the present invention through n- dodecyl mereaptan (NDM) Passivation Treatment Ge.
Embodiment
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate the present invention
Rather than limitation the scope of the present invention.In addition, it is to be understood that after the content of the invention lectured has been read, people in the art
Member can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited
Scope.
Embodiment 1
The mercaptan for being used to be passivated in the present embodiment is n- dodecyl mereaptan (molecular formula CH3(CH2)10CH2SH, english abbreviation is
NDM), the Ge pieces crystal orientation for treating Passivation Treatment is (111).
As shown in figure 1, comprising the following steps：
Step 1：The small pieces for being 5mm × 5mm for the Ge pieces cutting of (111) by crystal orientation, are then dipped into third successively by Ge pieces
It is cleaned by ultrasonic 15min in ketone and ethanol solution to remove the organic pollution on Ge pieces surface.Ge prints nitrogen after ultrasonic cleaning
Drying is stand-by.
Step 2：Ge pieces after surface cleaning processing in step 1 are dipped into 30min in deionized water, it is preliminary to remove Ge pieces
Water miscible oxide (such as GeO on surface2).Then Ge pieces are dipped into the hydrochloric acid solution that mass percent is 10% and soaked
30min is handled, the oxide of Ge piece remained on surface is further removed.Then with after enough deionized water rinsing HCl treatments
Ge samples, obtain the Ge samples of surface chlorination after being dried up with nitrogen.
Step 3：The n- dodecyl mereaptan solution 10mL for being 2ammol/L with absolute ethyl alcohol compound concentration, is sufficiently mixed backward molten
10mL deionized water is added in liquid.To ensure that reagent mixing is abundant, reagent is sufficiently mixed with oscillator until in mix reagent
White suspended things disappear.(second alcohol and water is by volume for the n- dodecyl mereaptan solution that the reaction reagent finally given is ammol/L
1:1 prepares).The n- dodecyl mereaptan for being respectively 0.1mmol/L, 1mmol/L and 10mmol/L according to above method compound concentration is anti-
Answer reagent.
Step 4：The Ge samples of the surface chlorination obtained in step 2 are dipped into the reaction for the various concentrations that step 3 is prepared
In reagent.To reduce the volatilization of ethanol in course of reaction, it is necessary to which reaction chamber is sealed.By sealed reaction chamber as 80 DEG C of baking
24h is reacted in case to obtain high-quality n- dodecyl mereaptan self-assembled monolayers.Reaction cleans Ge after terminating with EtOH Sonicate
Print can obtain the high-quality passivation in surface to remove n- dodecyl mereaptan molecule of the residual absorption on print surface after nitrogen drying
Ge pieces.This is tested other experimental implementations and carried out under room temperature (25 DEG C or so).
In the present embodiment, to illustrate the work with the difference and heating condition of conventional passivation method in passivating process
With devising two groups of control experiments herein.In control experiment one, the reaction temperature in step 4 is set as to carry out at room temperature,
Other experiment conditions are consistent with experimental group.Then the n- dodecyl mereaptan solution in step 3 is directly used in control experiment two
Absolute ethyl alcohol is prepared, and other experiment conditions are consistent with experimental group.
X-ray photoelectron power spectrum (XPS) result that Fig. 3 is Ge prints Ge3d before HCl treatment in the embodiment of the present invention,
Peak at 29.5eV corresponds to not oxidized simple substance Ge, and occurs peak at 32.8eV corresponding to sample surfaces self-assembling formation
Germanium oxide (GeOx), the result illustrates that the Ge sample surfaces before unused HCl treatment have natural oxidizing layer.
Fig. 4 be the embodiment of the present invention in after HCl treatment Ge prints Ge3d and Cl2p x-ray photoelectron power spectrum (XPS)
As a result, wherein Fig. 4 a Ge3d only has obvious peak value to occur at 29.5eV, and the peak at 32.8eV disappears and illustrated at hydrochloric acid
Reason effectively removes the oxide layer of Ge sample surfaces.And the bimodal explanation hydrochloric acid that Fig. 4 b Cl2p occurs in 198eV annexes is to Ge
There is the introducing of Cl atoms after print processing, so that Ge surface chlorinations.
The x-ray photoelectron power spectrum (XPS) that Fig. 5 is the C1s through n- dodecyl mereaptan Passivation Treatment Ge in the embodiment of the present invention
Comparative result result.Comparing result shows the experimental group (water content 50%, 80 DEG C) and control group (water content in embodiment
50%, 25 DEG C and not aqueous, 25 DEG C) phosphorus content be all higher than blank Ge prints, and the phosphorus content highest of experimental group.
The water contact angle stability comparing result that Fig. 6 is n- dodecyl mereaptan Passivation Treatment Ge in the embodiment of the present invention, the knot
The contact angle stability of the passivation Ge prints prepared in embodiment under different condition is compared in fruit.As a result aqueous conditions are shown in
Under the passivation protection effect of (water content 50%, 25 DEG C) be better than the result of traditional not aqueous (not aqueous, 25 DEG C), it is and further
The surface stability of passivation Ge prints can be greatly improved in appropriate heating (water content 50%, 80 DEG C), and test result shows the condition
Obtained Ge samples can for a long time (>10 days) keep its water contact angle to be more than 100 °, long-time monitoring result shows it in air
Stability under environment is more than 15 days.
Embodiment 2
The mercaptan for being used to be passivated in the present embodiment is positive 16 mercaptan (molecular formula CH3(CH2)15SH), treat at passivation
The Ge pieces crystal orientation of reason is (111).
As shown in figure 1, comprising the following steps：
Step 1：The organic pollution on Ge pieces surface is removed, detailed process is consistent with the step 1 in embodiment 1.
Step 2：Remove the oxide layer on Ge pieces surface and realize surface chlorination, detailed process is protected with the step 2 in embodiment 1
Hold consistent.
Step 3：The positive 16 thiol solution 10mL for being 2ammol/L with absolute ethyl alcohol compound concentration, is sufficiently mixed backward molten
10mL deionized water is added in liquid.To ensure that reagent mixing is abundant, reagent is sufficiently mixed with oscillator until in mix reagent
White suspended things disappear.(second alcohol and water is by volume for positive 16 thiol solution that the reaction reagent finally given is ammol/L
1:1 prepares).It is respectively 0.1mM, 1mM and 10mM positive 16 thiol reactant reagent according to above method compound concentration.
Step 4：The Ge samples of the surface chlorination obtained in step 2 are dipped into the reaction for the various concentrations that step 3 is prepared
In reagent.To reduce the volatilization of ethanol in course of reaction, it is necessary to which reaction chamber is sealed.By sealed reaction chamber as 80 DEG C of baking
24h is reacted in case to obtain high-quality positive 16 mercaptan self assembly molecular film.Reaction cleans Ge after terminating with EtOH Sonicate
Print can obtain the high-quality passivation in surface to remove positive 16 thiol molecule of the residual absorption on print surface after nitrogen drying
Ge pieces.This is tested other experimental implementations and carried out under room temperature (25 DEG C or so).
In the present embodiment, to illustrate the work with the difference and heating condition of conventional passivation method in passivating process
With devising two groups of control experiments herein.In control experiment one, the reaction temperature in step 4 is set as to carry out at room temperature,
Other experiment conditions are consistent with experimental group.Then positive 16 thiol solution in step 3 is directly used in control experiment two
Absolute ethyl alcohol is prepared, and other experiment conditions are consistent with experimental group.
Embodiment 3
The mercaptan for being used to be passivated in the present embodiment is positive stearylmercaptan (molecular formula CH3(CH2)17SH), treat at passivation
The Ge pieces crystal orientation of reason is (111).
As shown in figure 1, comprising the following steps：
Step 1：The organic pollution on Ge pieces surface is removed, detailed process is consistent with the step 1 in embodiment 1.
Step 2：Remove the oxide layer on Ge pieces surface and realize surface chlorination, detailed process is protected with the step 2 in embodiment 1
Hold consistent.
Step 3：The positive stearylmercaptan solution 10mL for being 2ammol/L with absolute ethyl alcohol compound concentration, is sufficiently mixed backward molten
10mL deionized water is added in liquid.To ensure that reagent mixing is abundant, reagent is sufficiently mixed with oscillator until in mix reagent
White suspended things disappear.(second alcohol and water is by volume for the positive stearylmercaptan solution that the reaction reagent finally given is ammol/L
1:1 prepares).It is respectively 0.1mM, 1mM and 10mM positive stearylmercaptan reaction reagent according to above method compound concentration.
Step 4：The Ge samples of the surface chlorination obtained in step 2 are dipped into the reaction for the various concentrations that step 3 is prepared
In reagent.To reduce the volatilization of ethanol in course of reaction, it is necessary to which reaction chamber is sealed.By sealed reaction chamber as 80 DEG C of baking
24h is reacted in case to obtain high-quality positive stearylmercaptan self-assembled monolayers.Reaction cleans Ge after terminating with EtOH Sonicate
Print can obtain the high-quality passivation in surface to remove positive stearylmercaptan molecule of the residual absorption on print surface after nitrogen drying
Ge pieces.This is tested other experimental implementations and carried out under room temperature (25 DEG C or so).
In the present embodiment, to illustrate the work with the difference and heating condition of conventional passivation method in passivating process
With devising two groups of control experiments herein.In control experiment one, the reaction temperature in step 4 is set as to carry out at room temperature,
Other experiment conditions are consistent with experimental group.Then the positive stearylmercaptan solution in step 3 is directly used in control experiment two
Absolute ethyl alcohol is prepared, and other experiment conditions are consistent with experimental group.
Particular embodiments described above, has been carried out further detailed to purpose of the present invention technical scheme and beneficial effect
Describe in detail it is bright, should be understood that the foregoing is only the present invention specific embodiment, be not intended to limit the invention, it is all
Within the spirit and principles in the present invention, any modification, equivalent substitution and improvements done etc., should be included in the guarantor of the present invention
Within the scope of shield.
Claims (6)
1. a kind of method of germanium material surface-stable passivation, it is characterised in that：Comprise the following steps that：
(1) Ge pieces are sequentially placed into acetone and ethanol solution and be cleaned by ultrasonic；
(2) soaking and washing is carried out to Ge pieces using deionized water and hydrochloric acid solution successively；
(3) it is formulated for the thiol solution of passivation；Wherein, thiol solution concentration is 0.1~10mmol/L, and solvent for use is ethanol
With the mixed liquor of water, the percent by volume of its reclaimed water is 10~50%；
Passivation Treatment in thiol solution will be dipped at (4) 60~80 DEG C with cleaned Ge pieces, you can.
2. a kind of method of germanium material surface-stable passivation according to claim 1, it is characterised in that：The step (1)
In Ge pieces be crystal orientation (100), (110) or (111) Ge pieces, or the Ge to grow on insulating barrier.
3. a kind of method of germanium material surface-stable passivation according to claim 1, it is characterised in that：The step (2)
The mass percent of middle hydrochloric acid is 5~10%.
4. a kind of method of germanium material surface-stable passivation according to claim 1, it is characterised in that：The step (2)
The processing time of middle deionized water and hydrochloric acid is 30min~2h.
5. a kind of method of germanium material surface-stable passivation according to claim 1, it is characterised in that：The step (3)
Middle mercaptan CH3(CH2)nSH contains Long carbon chain, n >=9.
6. a kind of method of germanium material surface-stable passivation according to claim 1, it is characterised in that：The step (4)
The middle Passivation Treatment time is 12~24h, the sealing of passivation reaction system.
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| CN104985177B (en) * | 2015-06-18 | 2017-05-17 | 南开大学 | Method for preparing nanometer germanium particles with passivated surfaces |
| US10290505B2 (en) | 2015-08-14 | 2019-05-14 | Entegris, Inc. | Passivation of germanium surfaces |
| CN107706088A (en) * | 2017-09-08 | 2018-02-16 | 吉林建筑大学 | A kind of semiconductor material surface wet method passivating method |
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| WO2011156019A2 (en) * | 2010-02-25 | 2011-12-15 | Merck Patent Gmbh | Group iv metal or semiconductor nanowire fabric |
| CN102005390B (en) * | 2010-10-19 | 2012-10-17 | 复旦大学 | Surface passivation method for Ge |
| CN103681245A (en) * | 2013-12-26 | 2014-03-26 | 中国科学院微电子研究所 | Method for cleaning germanium sheet and passivating surface of germanium sheet |
| CN103700581A (en) * | 2013-12-26 | 2014-04-02 | 中国科学院微电子研究所 | Method for manufacturing metal and n-type semiconductor germanium source drain contact |
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