CN105057691B - The method for mixing the substrate surface deposition nanogold particle of self-assembled molecule layer modification - Google Patents
The method for mixing the substrate surface deposition nanogold particle of self-assembled molecule layer modification Download PDFInfo
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Abstract
The invention discloses a kind of method for the substrate surface deposition nanogold particle for mixing self-assembled molecule layer modification, this method includes：The surface of oxide or inorganic substrates will be subjected to clean processing, remove the organic matters such as grease, the greasy dirt of silicon face, inorganic matter and oxide layer, make substrate surface hydroxylating；The method of fractional steps then is used, is immersed in pretreated silicon base in the solution containing organosilan self assembly molecule, silicon face molecular self-assembling modification is carried out, obtains the self assembled monolayer of different organic chain mixed growths；Finally the substrate surface for having mixing self assembled monolayer is being grown using citrate method deposition gold nano grain.Substrate cleaning method and method of modifying can be realized to the equally distributed regulation and control of gold nano grain by the growth time of self assembly molecule used according to the present invention, the gold nano grain being evenly distributed can be prepared, its particle diameter is well bonded up to 10~100nm between nanogold particle and substrate.
Description
Technical field
Present invention design belongs to surface modification field, and in particular to a kind of surface treatment of silicon base, more particularly, to one
The method of the film modified substrate surface deposition nanogold particle of kind molecular self-assembling.
Background technology
Now, electromechanical devices gradually develop to miniaturization, intelligent, multifunctional integrated direction.And it is used as extensive
The monocrystalline silicon of one of important semi-conducting material applied to integrated circuit, because it has metalloid physical property, significant
Semiconduction, it is allowed to be constantly in the forward position of new energy development.
Because monocrystalline silicon is widely used in microsystem, but the limitation of homogenous material performance causes in silicon substrate surface
The research of the composite organic alkane self-assembled film of growth turns into focus, especially with the functional group on molecular self-assembled monolayer surface,
The Organic-inorganic composite self-assembled film of inorganic nano-particle is assembled because its superior photoelectricity, wear-resistant, catalytic performance etc. are even more
By extensive concern.In Organic-inorganic composite self-assembled film system, golden nanometer particle is because of its unique optics, electronic catalytic
Can, and chemical stability is good, is easily-synthesized as the research hot topic in the fields such as chemical biosensor, microsystem friction.
Preparing the method for gold nano grain at present has many kinds to include compound electric deposition method, ion plating, sputtering and liquid phase side
The power consumption of method, wherein compound electric deposition method, ion plating, sputtering etc. is high, preparation condition requires high physical method；And for liquid phase
Synthetic method is learned, due to the small-size effect of nano particle, high surface free energy property makes the nano particle of liquid phase synthesis easily produce
It is raw to reunite.With regard to industry at present on silicon materials for the processing mode of depositing metal particles, be largely by evaporation coating and
The sputter coating such as dry method depositional mode such as chemical vapor deposition, magnetron sputtering, outside deposition metal target, cavity inner wall is subsidiary
Deposit can cause cost to waste.And electrodeposition process synthesizing nano-particle, then technique is coarse, the pattern of nano particle, size, point
Cloth uniformity is not easily-controllable.
The self-assembling technique occurred in currently available technology is a kind of under gentle simple condition, utilizes chemical bond
Metallic is bonded in substrate surface by bonding, and uses self-assembling technique to deposit the good soft metal of the self-lubricating properties such as gold
In substrate surface, can avoid using the physics side that the power consumption such as compound electric deposition method, ion plating, sputtering is high, preparation condition requirement is high
Method.
In terms of having had some researchs at present by growth of the self-assembling technique applied to gold nano grain deposition, utilization is organic
Functional group's (such as sulfydryl, carboxyl) in molecule in intermetallic chemical reaction, can Mouding metal nanoparticle be deposited on from
Assemble in film modified substrate.Such as Chinese patent literature (Publication No. CN 102978592A) discloses a kind of silicon face wet method
The method for depositing gold nano grain, the method wet-cleaning method such as boil using organic solution and handle silicon substrate surface, and use is single
The self-assembled film modification silicon substrate surface of component, and gold nano grain is deposited with wet chemical method, still, one-component from group
Molecular film is filled for regulating and controlling the distribution density of gold nano grain and insensitive, it is impossible to be preferably evenly distributed on gold nano grain
Substrate surface, and many hazardous solvents be present in cleaning way therein, it is larger to human body environment's injury, easily wash bad substrate.
The content of the invention
It is the defects of for prior art, a kind of by self-assembled monolayers modified substrate it is an object of the invention to propose
Method prepares gold nano grain, independently fill technology using molecule so that the sulfydryl (- SH) that can be chemically bonded with gold ion and
The different functional groups that can not be chemically bonded with gold ion uniformly generate in monocrystal silicon substrate Dispersion on surface, so as to pass through the party
Method prepares the nanogold particle of deposition, can solve the problem that the problem of gold nano grain is easily reunited in deposition.
The present invention proposes a kind of method for the substrate surface deposition nanogold particle for mixing self-assembled molecule layer modification, its
It is characterised by, this method comprises the following steps：
1) by the clean processing of substrate surface, removing surface oxide layer simultaneously makes surface hydroxylation；
2) prepare mixing self-assembled molecule layer and modify the substrate surface, making it have can be chemically bonded with gold ion
And the different functional groups that can not be chemically bonded with gold ion；
3) electronation deposition gold nano grain.
Further, in the step 1), the method for the clean processing of the substrate surface is cleaned for plasma oxygen.
Further, the time range of the plasma oxygen cleaning is 1-5 minutes.
Further, substep prepares the function that can be chemically bonded in silicon face generation with metal in the step (2)
Group and the functional group that can not be chemically bonded with metal.
Further, the method for the functional group that the self assembly can be chemically bonded with metal is that silicon chip is immersed into afterbody
Group is the organo silane coupling agent solution of sulfydryl.
Further, the method for the functional group that the self assembly can not be chemically bonded with metal is that silicon chip is immersed into band
There is the solution of one or more of mixing in methyl, alkenyl or carbonyl group.
Further, the time range of the immersion is 1-30 minutes.
Further, the time range of the immersion is 6-24 hours.
In addition, the invention also provides a kind of preparation method for mixing self-assembled molecule layer modification substrate, this method includes
Following steps：
1) oxide or inorganic substrates clean surface are handled, removes surface oxide layer and make surface hydroxylation；
2) prepare mixing self-assembled molecule layer and modify the substrate surface, chemical bond can be occurred with metal ion by making it have
Different functional groups closing and can not being chemically bonded with metal ion.
According to the method for preparing gold nano grain using the substrate of mixed self assembled monolayers modification of the present invention, can obtain such as
Lower advantage：
(1) present invention employs the mode of two-component self-assembled monolayers modification silicon base to prepare gold nano grain, by
In molecular self-assembled monolayer carried out by the chemical absorption of surface reaction from limitation, when silicon chip immerses the solution of the molecule containing assembling
Between difference, the state of its organic molecule Absorption Growth is different, is a work that can control gold nano grain distribution density
Skill technology；
(2) because substrate is by the way of plasma cleaning, surface grease organic matter and oxidation can effectively be removed
Thing, reach surface hydroxylation；Wet-cleaning is contrasted, it is not only simple to operate, the time is short, efficiency high, organic solvent can also be reduced
Use；
(3) present invention is prepared using based on wet method gold nano grain, and liquid phase method can be avoided to prepare the group of nano particle appearance
Poly- phenomenon.
Brief description of the drawings
Fig. 1 is the flow chart for preparing gold nano grain structure according to the present invention；
Fig. 2 is the AFM shape appearance figures according to the gold nano grain prepared in embodiments of the invention four；
Fig. 3 is the AFM shape appearance figures according to the gold nano grain prepared in embodiments of the invention five；
Fig. 4 is the AFM shape appearance figures according to the gold nano grain prepared in embodiments of the invention six；
Fig. 5 is the change with octadecyl trichlorosilane alkane preparation time according to the nanogold particle coverage rate that the present invention realizes
Tendency chart.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with drawings and Examples
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.
Wherein, as shown in figure 1, according to the present invention the silicon base film modified in molecular self-assembling on prepare gold nano grain
The flow chart of structure, certainly, the substrate are specifically not limited to silicon, but can be metal oxide or inorganic substrates, such as
Aluminum oxide, zinc oxide etc.；Inorganic substrates can be glass, mica sheet etc., can be grown in above substrate, wherein preparing nanometer
Gold grain comprises the following steps that：
(1) silicon chip surface is subjected to plasma oxygen gas disposal, removes surface oxide layer and make surface hydroxylation；
The general principle of molecular self-assembled monolayer is flim forming molecule in substrate surface, formed chemical bond linkage, arrangement closely,
It is orientated consistent Ordered Film.Organosilan quasi-molecule, facile hydrolysis, be condensed with the silicone hydroxyl of substrate surface, formed Si-O-Si keys with
Substrate is combined, and the two-dimension netted polysilane film of high quality is formed in hydroxylated surface.The shape of organosilan self-assembled monolayer
Associated factor into quality is a lot, such as solution concentration, temperature, humidity, substrate cleaning degree etc., the clean-up performance of substrate surface
And surface hydroxylation quality can directly affect water adsorptivity and organosilane molecules substrate surface absorption, hydrolysis, polymerization
Reaction, is the key link for preparing dense regular self-assembled film.If substrate can not be preferably covered with reaction active groups hydroxyl, meeting
So that self-assembled film produces defect, strand collapses or oriented is inconsistent.
And the cleaning way for the plasma that the present invention uses, the influence index involved by it is mainly cleaning way and cleaning
Time, the plasma cleaning of short time can make substrate surface cleaning and hydroxylating, but cleaning can injure substrate table for a long time excessively
Face, cause " secondary pollution " of cleaning, and select the plasma of reactant gas, for example, oxygen, the active particle being excited
Superficial layer can be made to produce a large amount of free radical hydroxyls, change the time model of the wetability of substrate surface, the wherein cleaning of plasma oxygen
Enclose for 1-5 minutes, the time is too short can not to clean up substrate surface, and overlong time causes the wasting of resources.
By using octadecyl trichlorosilane alkane, n-octyl silane, octadecyl trimethoxysilane and (3- sulfydryls third
Base) silicon substrate surface of organic coupling agent after the pre-treatment such as trimethoxy silane grows mixing self assembled monolayer, from
And substrate surface is modified.
Because the mixing self assembled monolayer of growth has different functional groups, both functional groups can be with metal
The hydrophobic grouping learned the sulfydryl (- SH) of bonding and be not easy to be chemically bonded with metal can be rolled into a ball including methyl (- CH3), removed certainly
Outside methyl, also alkenyl, carbonyl etc. these be all not easy and metal bonding, the site with mercapto functional group is to allow
The site that gold nano grain chemically reacts with it, it is other that gold nano is hindered by the place covered containing methyl organic chain
The deposition of grain, such wet chemistry synthesis gold nano grain can be deposited on silicon substrate by being reacted with particular functional group and more uniform
Basal surface.
The present invention obtains the homogeneous organic self-assembled molecule layer of mixing using modification is carried out to silicon base, due to organosilicon
Alkane, can be in hydroxylated superficial growth, and other oxide surfaces after plasma cleaning are respectively provided with equally distributed hydroxyl,
Therefore this method of modifying can adapt in the modification of the surface of oxide base, and the wherein material of oxide base can be oxidation
Silicon or aluminum oxide etc..
Embodiment one
1) by the clean processing of silicon chip surface, removing surface oxide layer simultaneously makes surface hydroxylation；
It is described that the clean processing of silicon chip surface, removing surface oxide layer are simultaneously made into the specific of surface hydroxylation in step 1)
Step is as follows：
A the silicon chip of specification carries out plasma cleaning in plasma cleaner with oxygen needed for) being cut into, and scavenging period is
It is standby to take out silicon chip for 2min, then sealing；
2) method of fractional steps prepares mixing self-assembled molecule layer modification silicon face；
In step 2), the method for fractional steps prepares comprising the following steps that for mixing self-assembled molecule layer modification silicon face：
B) by through step A) to be directly immersed in molar concentration be 10mmol/L octadecyl trichlorosilanes for silicon materials after processing
1min in the toluene solvant of alkane, wherein toluene are treated dry toluene, and time of repose is 10min~30min, is obtained in silicon
The self assembly organic monolayer of the unsaturated growth of piece surface octadecyl trichlorosilane alkane.Whole octadecyl trichlorosilane alkane is from group
The preparation process of monolayer is filled in nitrogen (N2) or the protection of argon gas (Ar) atmosphere, exclusion of water and oxygen room temperature environment in carry out；
C silicon chip) is taken out, first with 5~10min of dry toluene rinse；Then acetone 5~10min of rinse is used, fully to clean
Decorating molecule of the physical absorption in silicon face；Finally dried up with nitrogen；
D) by through step C) to be directly immersed in molar concentration be 5mmol/L (3- mercaptopropyis) front three for silicon materials after processing
In the anhydrous ethanol solvent of TMOS, time of repose 24h, to ensure that the growth of its saturation reduces defect generation, obtain in silicon
The self assembly organic molecule of octadecyl trichlorosilane alkane/(3- mercaptopropyis) trimethoxy silane that the mixing of piece surface homogeneously grows
Layer.Entirely the preparation process of (3- mercaptopropyis) trimethoxy silane self assembled monolayer is equally in nitrogen (N2) or argon gas
(Ar) carried out in the room temperature environment of atmosphere protection, exclusion of water and oxygen；
E silicon chip) is taken out, first with 5~10min of absolute ethyl alcohol rinse；Then acetone 5~10min of rinse is used, fully to clean
Decorating molecule of the physical absorption in silicon face；Finally dried up with nitrogen；
When silicon chip is immersed in the toluene solvant of octadecyl trichlorosilane alkane (ODTS) after processing, ODTS molecules are rapidly and base
Hydroxyl reaction on bottom, but partial hydrolysis can only occur in the short time, ODTS molecule of the physical absorption in substrate surface is cleaned, with
After be immersed in MPTS solution, there is larger hole in ODTS molecules, not fine and close with intermolecular；MPTS just with the ODTS in substrate
Hydroxyl reaction at molecular gap.
3) electronation deposition gold nano grain；
F step E will) be passed through) modified and the silicon base cleaned carry out citrate reduction method deposition gold nano grain, and it is real
Existing silicon face gold nano grain uniform deposition；The chemical reaction liquid of the citrate reduction method is gold salt-containing solution, citric acid
And the ultra-pure water solution of citrate, wherein gold salt-containing solution can be chlorauric acid solution, gold content 0.18g/L, take mole dense
Spend the chlorauric acid solution 5mL for 10mM/L to add in 100mL flasks with 45mL water, heating stirring is to 100 under the conditions of closed reflux
DEG C, keep adding the sodium citrate solution that 5mL molar concentrations are 40mM/L after 5min, room temperature be down to after persistently stirring 20min,
Solution is taken out to be kept in dark place.
G silicon chip) will have been modified it has been placed in 20ml solution and be maintained at 28 degrees Celsius of lower 1h, has surpassed in deionized water after taking-up
Sound 5min, nitrogen drying, is kept in dark place afterwards.
By same steps " one, silicon base cleaning treatment, and hydroxylating handle ", different built-up times processing embodiment
Referring to table 1
Table 1 mixes the contrast table of the different built-up times of self-assembled modified substrate surface
In above-mentioned preparation process, step 2) surface should be carried out immediately after the processing of step 1) silicon chip surface cleaning hydroxylating
Molecular self-assembling grows, it is impossible to which time of occurrence pauses.
Chemical reagent employed in above-mentioned preparation process is to analyze pure and above purity, when configuring solution, is used
Water is ultra-pure water.
In a further embodiment, distribution can be directly obtained on the silicon substrate surface after modification through overtesting, this method
Uniformly, the controllable gold nano grain of density, grain diameter are 10nm~30nm.Wherein, as shown in Fig. 2 being realized for example IV
Assembled again after silicon substrate surface grows 1min octadecyl trichlorosilane alkanes 6h (3- mercaptopropyis) trimethoxy silane from
Monolayer is assembled, then carries out the AFM figures that citric acid reduction deposition gold nano grain obtains, and as shown in figure 3, being embodiment
Five (3- mercaptopropyis) trimethoxies for assembling 6h again after silicon substrate surface grows 10min octadecyl trichlorosilane alkanes realized
Silane self assembled monolayer, then carry out the AFM figures that citric acid reduction deposition gold nano grain obtains, it is seen that gold nano grain
Be evenly distributed, particle size it is more consistent.And what embodiment six was realized grows 30min octadecyl trichlorosilane alkanes in silicon substrate surface
Assemble 6h (3- mercaptopropyis) trimethoxy silane self assembled monolayer again afterwards, then carry out citric acid reduction deposition Jenner
The AFM figures that rice grain obtains, as shown in Figure 4, it can be seen that gold nano grain number is reduced in figure, but particle size, distribution density
Also than more uniform.Gold nano grain can be adjusted in silicon chip by component growth time in control mixing self-assembled molecule layer
On settled density, influence of the growth time for gold grain be because substrate surface covering group ratio difference caused by.
When the first organic molecular species grow, the length of time can control it in the coverage rate of silicon chip substrate surface, and its own can be because
For growth time is unsaturated defect is produced, when then carrying out second of self assembly molecule growth, it will not be filled
Region growing, so density can have any different, and the sulfydryl of second of molecule afterbody can be bonded with metal, result in gold
The density of grain is different.Generally, the figure established according to growth time as shown in figure 5, the distribution of particles figure of different preparation times, its
Grain density is different, and respectively 68.8%, 36.2%, 31.6%, 27%, the above results demonstrate effectiveness of the invention, can
Row and controllability.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to
The limitation present invention, all any modification, equivalent and improvement made within the spirit and principles of the invention etc., all should be included
Within protection scope of the present invention.
Claims (3)
1. a kind of method for the substrate surface deposition nanogold particle for mixing self-assembled molecule layer modification, this method include following step
Suddenly：
1) by the clean processing of substrate surface, removing surface oxide layer simultaneously makes surface hydroxylation；
2) mixing self-assembled molecule layer is prepared using the method for fractional steps and modifies the substrate surface, making it have can occur with metal ion
Different functional groups that are chemical bonding and can not being chemically bonded with metal ion, wherein, formation can occur with metal ion
The method of the functional group of chemical bonding be by silicon chip immersion tail groups be sulfydryl organo silane coupling agent solution, immersion when
Between scope be 6-24 hours；The method for forming the functional group that can not be chemically bonded with metal ion is to immerse silicon chip to carry
The solution of one or more of mixing in methyl, alkenyl or carbonyl group, the time range of immersion is 1-30 minutes；
3) electronation deposition gold nano grain.
2. the method for the substrate surface deposition nanogold particle of mixing self-assembled molecule layer modification as claimed in claim 1, its
It is characterised by the step 1), the method for the clean processing of the substrate surface is cleaned for plasma oxygen.
3. the method for the substrate surface deposition nanogold particle of mixing self-assembled molecule layer modification as claimed in claim 2, its
It is characterised by, the time range of the plasma oxygen cleaning is 1-5 minutes.
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| CN108529553B (en) * | 2017-09-22 | 2020-02-18 | 中北大学 | Graphene high-temperature pressure sensor packaging method |
| US10607832B2 (en) * | 2018-01-15 | 2020-03-31 | Samsung Electronics Co., Ltd. | Method and apparatus for forming a thin layer |
| CN108467009A (en) * | 2018-03-06 | 2018-08-31 | 西安交通大学 | A method of utilizing the controllable SWNT scale arrays of Chemical self-assembly manufacture line width |
| CN108972319A (en) * | 2018-09-18 | 2018-12-11 | 长鑫存储技术有限公司 | Chemical and mechanical grinding cushion and preparation method thereof |
| CN109580650B (en) * | 2018-12-14 | 2021-06-25 | 清华大学 | Method for detecting surface cleanliness of graphene |
| CN110724908A (en) * | 2019-11-18 | 2020-01-24 | 合肥安德科铭半导体科技有限公司 | Method for modifying surface of inorganic substance substrate |
| CN111793476B (en) * | 2020-07-09 | 2022-01-25 | 深圳先进电子材料国际创新研究院 | Heat conduction material and preparation method thereof |
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| CN1485377A (en) * | 2002-09-25 | 2004-03-31 | 东南大学 | Self-assembly process for nano corrosion-proof film on the metal surface |
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| CN102828176A (en) * | 2012-07-31 | 2012-12-19 | 东南大学 | Preparation method for uniform gold nanoparticle film |
| CN102978592A (en) * | 2012-12-24 | 2013-03-20 | 厦门大学 | Method for depositing gold nanoparticles on silicon surface by wet process |
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| GB2463878A (en) * | 2008-09-25 | 2010-03-31 | Dca Consultants Ltd | Ionic catalyst capture of carbon oxides |
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