CN105057691A - Method for sedimentating nanogold particles on substrate surface modified with mixed self-assembly molecular layer - Google Patents
Method for sedimentating nanogold particles on substrate surface modified with mixed self-assembly molecular layer Download PDFInfo
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Abstract
The invention discloses a method for sedimentating nanogold particles on a substrate surface modified with a mixed self-assembly molecular layer. The method comprises the following steps that the surface of an oxide or an inorganic substrate is cleaned; grease, greasy dirt and other organic matter, inorganic matter and oxide layers are removed from a silicon surface, so that the surface of the substrate is hydroxylated; then a fractional step method is adopted; the pretreated silicon substrate is soaked in a solution containing organosilane self-assembly molecules and molecular self-assembly modification on the silicon surface is carried out; self-assembly monomolecular layers with mixed growth of various organic chains are obtained; and at last, a citrate method is adopted for sedimentating gold nanoparticles on the substrate surface grown with a mixed self-assembly monomolecular layer. According to the method, a substrate cleaning method and a modification method can achieve regulation and control over the even distribution of the gold nanoparticles through the growth time of self-assembly molecules; the gold nanoparticles distributed evenly can be prepared and the grain size of the gold nanoparticles is between 10-100 nm; and the gold nanoparticles can be combined well with the substrate.
Description
Technical field
The present invention's design belongs to finishing field, is specifically related to a kind of surface treatment of silicon base, especially relates to the method for the film modified substrate surface depositing nano gold grain of a kind of molecular self-assembling.
Background technology
Now, electromechanical devices is gradually to microminiaturized, intelligent, multifunctional integrated future development.And as the monocrystalline silicon of one of the important semi-conducting material being widely used in integrated circuit, because it has metalloid physical property, significant semiconduction, make it the forward position being always in new forms of energy development.
Because monocrystalline silicon is widely used in microsystem, but the limitation of homogenous material performance makes the research of the composite organic alkane self-assembled film in silicon substrate surface growth become focus, especially utilize the functional group on molecular self-assembled monolayer surface, assemble the Organic-inorganic composite self-assembled film of inorganic nano-particle because of its superior photoelectricity, resistance to wear, catalytic performance etc. is especially by extensive concern.In Organic-inorganic composite self-assembled film system, golden nanometer particle is because of optics, the electronic catalytic performance of its uniqueness, and the research that good, the easy synthesis of chemical stability becomes the field such as chemical biosensor, microsystem friction is popular.
The method preparing gold nano grain at present has and a variety ofly comprises compound electric deposition method, ion plating, sputtering and liquid phase process, and wherein high, the preparation condition of the power consumption such as compound electric deposition method, ion plating, sputtering requires high physical method; And for chemical synthesis in liquid phase method, due to the small-size effect of nano particle, high surface free energy character makes the nano particle of liquid phase synthesis easily produce reunion.With regard to the processing mode of current industry depositing metal particles on silicon materials, major part is as the dry method such as chemical vapour deposition (CVD), magnetron sputtering depositional mode by evaporation coating and sputter coating, outside deposition metal target, the subsidiary deposit of cavity inner wall can cause cost to waste.And electrodeposition process synthesizing nano-particle, then technique is coarse, and the pattern of nano particle, size, distributing homogeneity are not easily controlled.
The self-assembling technique occurred in currently available technology is a kind of under gentle simple condition, utilize the bonding of chemical bond that metallic is bonded in substrate surface, and use self-assembling technique soft metal good for the self-lubricating properties such as gold to be deposited on substrate surface, can avoid using the physical methods that power consumption is high, preparation condition requirement is high such as compound electric deposition method, ion plating, sputtering.
Some researchs have been had self-assembling technique to be applied to the growth aspect of gold nano grain deposition at present, utilize the functional group in organic molecule (as sulfydryl, carboxyl etc.) in intermetallic chemical reaction, can be deposited in the substrate of self-assembled film modification by Mouding metal nanoparticle.Such as Chinese patent literature (publication number is CN102978592A) discloses a kind of method of silicon face wet method deposited gold nano particle, this method wet-cleaning method process silicon substrate surface such as utilize organic solution to boil, the self-assembled film of one-component is adopted to modify silicon substrate surface, and with wet chemical method deposited gold nano particle, but, the self-assembled monolayers of one-component is insensitive for the distribution density of regulation and control gold nano grain, can not gold nano grain be made preferably to be evenly distributed on substrate surface, and there is a lot of hazardous solvent in cleaning way wherein, larger to human body environment's injury, easily wash bad substrate.
Summary of the invention
For the defect of prior art, the object of the invention is to propose a kind of method by self-assembled monolayers modified substrate and prepare gold nano grain, the autonomous packing technique of molecule is utilized to make with the sulfydryl (-SH) of gold ion generation chemical bonding and evenly can not to generate at monocrystal silicon substrate Dispersion on surface with the different functional groups of gold ion generation chemical bonding, thus by the nanogold particle that the method preparation deposits, the problem that gold nano grain easily occurs to reunite in deposition can be solved.
The present invention proposes a kind of method mixing the substrate surface depositing nano gold grain that self-assembled molecule layer is modified, it is characterized in that, the method comprises the steps:
1) by substrate surface cleaning process, removing surface oxide layer also makes surface hydroxylation;
2) preparation mixing self-assembled molecule layer modify described substrate surface, make it have can with gold ion generation chemical bonding and can not with the different functional groups of gold ion generation chemical bonding;
3) electronation deposited gold nano particle.
Further, described step 1) in, the method for described substrate surface cleaning process is the cleaning of plasma oxygen.
Further, the time range of described plasma oxygen cleaning is 1-5 minute.
Further, in described step (2) substep be prepared in silicon face generate can with the functional group of metal generation chemical bonding with can not with the functional group of metal generation chemical bonding.
Further, described self assembly can be silicon chip is immersed the organo silane coupling agent solution that tail groups is sulfydryl with the method for the functional group of metal generation chemical bonding.
Further, described self assembly can not be immerse silicon chip with one or more solution mixed in methyl, thiazolinyl or carbonyl group with the method for the functional group of metal generation chemical bonding.
Further, the time range of described immersion is 1-30 minute.
Further, the time range of described immersion is 6-24 hour.
In addition, the invention allows for a kind of preparation method mixing self-assembled molecule layer modification substrate, the method comprises the steps:
1) by oxide or the process of inorganic substrates clean surface, removing surface oxide layer also makes surface hydroxylation;
2) preparation mixing self-assembled molecule layer modify described substrate surface, make it have can with metal ion generation chemical bonding and can not with the different functional groups of metal ion generation chemical bonding.
Prepare the method for gold nano grain according to the substrate utilizing mixed self assembled monolayers to modify of the present invention, following advantage can be obtained:
(1) present invention employs the mode at two component self-assembled monolayers modified silicon based end to prepare gold nano grain, because molecular self-assembled monolayer is undertaken by the chemical absorption of surface reaction from restriction, silicon chip immerses the difference of the solution min containing assembling molecule, the state of its organic molecule Absorption Growth is different, is a technology that can control gold nano grain distribution density;
(2) because substrate is the mode adopting plasma cleaning, effectively can remove surperficial grease organic matter and oxide, reach surface hydroxylation; Contrast wet-cleaning, not only simple to operate, the time is short, efficiency is high, can also reduce the use of organic solvent;
(3) the present invention uses based on the preparation of wet method gold nano grain, can avoid the agglomeration that Liquid preparation methods nano particle occurs.
Accompanying drawing explanation
Fig. 1 is according to the flow chart preparing gold nano grain structure of the present invention;
Fig. 2 is the AFM shape appearance figure according to the gold nano grain of preparation in embodiments of the invention four;
Fig. 3 is the AFM shape appearance figure according to the gold nano grain of preparation in embodiments of the invention five;
Fig. 4 is the AFM shape appearance figure according to the gold nano grain of preparation in embodiments of the invention six;
Fig. 5 is that the nanogold particle coverage rate that realizes according to the present invention is with the changing trend diagram of octadecyl trichlorosilane alkane preparation time.
Detailed description of the invention
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
Wherein, as shown in Figure 1, according to flow chart gold nano grain structure preparing by the silicon base film modified at molecular self-assembling of the present invention, certainly, this substrate is not specifically defined as silicon, but can be metal oxide or inorganic substrates, such as aluminium oxide, zinc oxide etc.; Inorganic substrates can be glass, mica sheet etc., can grow in above substrate, and the concrete steps wherein preparing nanogold particle are as follows:
(1) silicon chip surface is carried out plasma oxygen gas disposal, removing surface oxide layer also makes surface hydroxylation;
The general principle of molecular self-assembled monolayer be flim forming molecule at substrate surface, formed chemical bond linkage, arrangement closely, Ordered Film that orientation is consistent.Organosilan quasi-molecule, facile hydrolysis, with the silicone hydroxyl condensation of substrate surface, forms Si-O-Si key and is combined with substrate, form high-quality two-dimension netted polysilane film at hydroxylated surface.The factor that is associated of the formation quality of organosilan self-assembled monolayer is a lot, such as solution concentration, temperature, humidity, substrate cleaning degree etc., the clean-up performance of substrate surface and surface hydroxylation quality directly can affect the adsorptivity of water and organosilane molecules in the absorption of substrate surface, hydrolysis, polymerisation, are the key links preparing dense regular self-assembled film.If substrate can not better be coated with reaction active groups hydroxyl, can make self-assembled film produce defect, strand collapse or oriented inconsistent.
And the isoionic cleaning way that the present invention adopts, influence index involved by it is cleaning way and scavenging period mainly, the plasma cleaning of short time can make substrate surface clean and hydroxylating, but cross long-time cleaning and can injure substrate surface, cause " secondary pollution " of cleaning, and select the plasma of reactant gas, such as oxygen, the active particle be excited can make superficial layer produce a large amount of free radical hydroxyl, change the wetability of substrate surface, wherein the time range of plasma oxygen cleaning is 1-5 minute, time is too short cannot clean up substrate surface, overlong time causes the wasting of resources.
By using the organic coupling agent silicon substrate surface after the pre-treatment such as octadecyl trichlorosilane alkane, n-octyl silane, octadecyl trimethoxysilane and (3-mercaptopropyi) trimethoxy silane to grow mixing self assembled monolayer, thus modification is carried out to substrate surface.
Because the mixing self assembled monolayer of growth has different functional groups, this Liang Zhong functional group can roll into a ball with the sulfydryl (-SH) of metal generation chemical bonding and not easily with the hydrophobic grouping of metal generation chemical bonding and comprise methyl (-CH3), certainly except methyl, also has thiazolinyl, carbonyl etc. these all not easily with metal bonding, namely the site with mercapto functional group is to allow the site of gold nano grain and its generation chemical reaction, other is hindered the deposition of gold nano grain by the place covered containing methyl organic chain, namely such wet chemistry synthesis gold nano grain is deposited on silicon substrate surface more uniformly by reacting with particular functional group.
The present invention uses and carries out modifying the organic self-assembled molecule layer obtaining mixing homogeneous phase to silicon base, due to organosilan, can in hydroxylated superficial growth, and other oxide surfaces after plasma cleaning all have equally distributed hydroxyl, therefore this method of modifying can be adapted to the surface modification of oxide base, and wherein the material of oxide base can be silica or aluminium oxide etc.
Embodiment one
1) by silicon chip surface cleaning process, removing surface oxide layer also makes surface hydroxylation;
In step 1) in, described by silicon chip surface cleaning process, removing surface oxide layer also makes the concrete steps of surface hydroxylation as follows:
A) silicon chip being cut into required specification is carried out plasma cleaning with oxygen in plasma cleaner, scavenging period is 2min, and it is for subsequent use that silicon chip is taken out in sealing subsequently;
2) method of fractional steps preparation mixing self-assembled molecule layer modifies silicon face;
In step 2) in, the concrete steps that described method of fractional steps preparation mixing self-assembled molecule layer modifies silicon face are as follows:
B) by through steps A) to be directly immersed in molar concentration be 1min in the toluene solvant of 10mmol/L octadecyl trichlorosilane alkane for silicon materials after process, wherein toluene is the dry toluene processed, time of repose is 10min ~ 30min, obtains the self assembly organic monolayer in the unsaturated growth of silicon chip surface octadecyl trichlorosilane alkane.The preparation process of whole octadecyl trichlorosilane alkane self assembled monolayer is at nitrogen (N
2) or the protection of argon gas (Ar) atmosphere, exclusion of water and oxygen room temperature environment in carry out;
C) take out silicon chip, first use dry toluene rinse 5 ~ 10min; Then acetone rinse 5 ~ 10min is used, fully to clean the decorating molecule that physics is adsorbed on silicon face; Finally dry up with nitrogen;
D) by through step C) to be directly immersed in molar concentration be in the anhydrous ethanol solvent of 5mmol/L (3-mercaptopropyi) trimethoxy silane for silicon materials after process, time of repose is 24h, to ensure that its saturated growth reduces defect and generates, obtain the self assembly molecule organic layer of octadecyl trichlorosilane alkane/(3-mercaptopropyi) trimethoxy silane in the growth of silicon chip surface mixing homogeneous phase.The preparation process of whole (3-mercaptopropyi) trimethoxy silane self assembled monolayer is equally at nitrogen (N
2) or the protection of argon gas (Ar) atmosphere, exclusion of water and oxygen room temperature environment in carry out;
E) take out silicon chip, first use absolute ethyl alcohol rinse 5 ~ 10min; Then acetone rinse 5 ~ 10min is used, fully to clean the decorating molecule that physics is adsorbed on silicon face; Finally dry up with nitrogen;
When after processing, silicon chip immerses in the toluene solvant of octadecyl trichlorosilane alkane (ODTS), ODTS molecule rapidly with suprabasil hydroxyl reaction, but can only generating portion be hydrolyzed in the short time, cleaning physics is adsorbed on the ODTS molecule of substrate surface, be immersed in MPTS solution subsequently, ODTS molecule and intermolecular existence comparatively macrovoid, not fine and close; MPTS just with the hydroxyl reaction at ODTS molecular gap place in substrate.
3) electronation deposited gold nano particle;
F) by through step e) modified the silicon base of cleaning carries out citrate reduction method deposited gold nano particle, realize silicon face gold nano grain uniform deposition; The chemical reaction liquid of described citrate reduction method is the ultra-pure water solution containing golden salting liquid, citric acid and citrate, wherein can be chlorauric acid solution containing golden salting liquid, gold content is 0.18g/L, get chlorauric acid solution 5mL that molar concentration is 10mM/L and 45mL water adds in 100mL flask, under closed reflux condition, heating is stirred to 100 DEG C, add the sodium citrate solution that 5mL molar concentration is 40mM/L after keeping 5min, after Keep agitation 20min, be down to room temperature, take out solution and keep in Dark Place.
G) be placed in 20ml solution remain on 28 degrees Celsius of lower 1h by having modified silicon chip, ultrasonic 5min in deionized water after taking-up, nitrogen dries up afterwards, keeps in Dark Place.
Through same steps " one, silicon base cleaning, and hydroxylating process ", the embodiment of different built-up time process is see 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, through step 1) should carry out step 2 immediately after the clean hydroxylating process of silicon chip surface) surface molecular self-assembled growth, can not pause by time of occurrence.
The chemical reagent adopted in above-mentioned preparation process is analyzes pure and above purity, and during configuration solution, the water of use is ultra-pure water.
In a further embodiment, through overtesting, the gold nano grain that this method can the silicon substrate surface after modified be directly evenly distributed, density is controlled, grain diameter is 10nm ~ 30nm.Wherein, as shown in Figure 2, for (3-mercaptopropyi) trimethoxy silane self assembled monolayer assembling 6h after silicon substrate surface growth 1min octadecyl trichlorosilane alkane again that embodiment four realizes, carry out the AFM figure that citric acid reduction deposited gold nano particle obtains subsequently, and as shown in Figure 3, for (3-mercaptopropyi) trimethoxy silane self assembled monolayer assembling 6h after silicon substrate surface growth 10min octadecyl trichlorosilane alkane again that embodiment five realizes, carry out the AFM figure that citric acid reduction deposited gold nano particle obtains subsequently, visible gold nano grain is evenly distributed, particle size is more consistent.And (3-mercaptopropyi) trimethoxy silane self assembled monolayer assembling 6h after silicon substrate surface growth 30min octadecyl trichlorosilane alkane again that embodiment six realizes, carry out the AFM figure that citric acid reduction deposited gold nano particle obtains subsequently, as shown in Figure 4, can see middle gold nano grain decreased number of publishing picture, but particle size, distribution density are also more even.Namely can regulate the settled density of gold nano grain on silicon chip by controlling component growth time in mixing self-assembled molecule layer, growth time is because the group ratio difference that substrate surface covers caused for the impact of gold grain.When the first organic molecule grows, the length of time can control its coverage rate at silicon wafer-based basal surface, it self can produce defect because growth time is unsaturated, when carrying out the growth of the second self assembly molecule subsequently, the region growing that it will not be filled, so density can be had any different, and the sulfydryl of the second molecule afterbody can with metal generation bonding, the density that result in gold grain is different.Generally, as shown in Figure 5, the distribution of particles figure of different preparation time, its grain density is different, and be respectively 68.8%, 36.2%, 31.6%, 27%, the above results demonstrates validity of the present invention, feasibility and controllability for the figure set up according to growth time.
Those skilled in the art will readily understand; the foregoing is only preferred embodiment of the present invention; not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (9)
1. mix a method for the substrate surface depositing nano gold grain that self-assembled molecule layer is modified, the method comprises the steps:
1) by substrate surface cleaning process, removing surface oxide layer also makes surface hydroxylation;
2) preparation mixing self-assembled molecule layer modify described substrate surface, make it have can with gold ion generation chemical bonding and can not with the different functional groups of gold ion generation chemical bonding;
3) electronation deposited gold nano particle.
2. the method for the substrate surface depositing nano gold grain of mixing self-assembled molecule layer as claimed in claim 1 modification, is characterized in that, described step 1) in, the method for described substrate surface cleaning process is the cleaning of plasma oxygen.
3. the method for the substrate surface depositing nano gold grain of mixing self-assembled molecule layer as claimed in claim 2 modification, is characterized in that, the time range of described plasma oxygen cleaning is 1-5 minute.
4. as the method for the substrate surface depositing nano gold grain of the mixing self-assembled molecule layer modification in claim 1-3 as described in any one, it is characterized in that, in described step (2) substep be prepared in silicon face generate can with the functional group of metal generation chemical bonding with can not with the functional group of metal generation chemical bonding.
5. the method for the substrate surface depositing nano gold grain of mixing self-assembled molecule layer as claimed in claim 4 modification, it is characterized in that, described self assembly can be silicon chip is immersed the organo silane coupling agent solution that tail groups is sulfydryl with the method for the functional group of metal generation chemical bonding.
6. the method for the substrate surface depositing nano gold grain of mixing self-assembled molecule layer as claimed in claim 5 modification, it is characterized in that, described self assembly can not be immerse silicon chip with one or more solution mixed in methyl, thiazolinyl or carbonyl group with the method for the functional group of metal generation chemical bonding.
7. the method for the substrate surface depositing nano gold grain of mixing self-assembled molecule layer as claimed in claim 5 modification, it is characterized in that, the time range of described immersion is 1-30 minute.
8. the method for the substrate surface depositing nano gold grain of mixing self-assembled molecule layer as claimed in claim 5 modification, it is characterized in that, the time range of described immersion is 6-24 hour.
9. mix the preparation method that self-assembled molecule layer modifies substrate, the method comprises the steps:
1) by oxide or the process of inorganic substrates clean surface, removing surface oxide layer also makes surface hydroxylation;
2) preparation mixing self-assembled molecule layer modify described substrate surface, make it have can with metal ion generation chemical bonding and can not with the different functional groups of metal ion generation chemical bonding.
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| CN109580650A (en) * | 2018-12-14 | 2019-04-05 | 清华大学 | A kind of detection method of graphene surface cleannes |
| 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 |
| CN111793476A (en) * | 2020-07-09 | 2020-10-20 | 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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