CN108258142A - A kind of method that ultrathin metal electrode is prepared based on molecular-layer deposition technology - Google Patents
A kind of method that ultrathin metal electrode is prepared based on molecular-layer deposition technology Download PDFInfo
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- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
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Abstract
A kind of method that ultrathin metal electrode is prepared based on molecular-layer deposition technology, belongs to optoelectronic device technology field.It is that substrate is heated to 100~300 DEG C in reaction chamber and keeps stable；Carrier gas is passed through after vacuumizing, makes cavity stable gas pressure in 0.1~0.3Torr；Then 0.02~20s presomas 1 are passed through into reaction chamber, 5~150s carrier gas is passed through and discharges extra presoma 1 and by-product；It is passed through 0.02~20s presomas 2 again, is passed through 5~150s carrier gas and discharges extra presoma 2 and by-product；Repeat that above step is multiple, so as to obtain the Seed Layer that the surface that thickness is 10~100nm has a large amount of regular chemical bonds in substrate surface；The super thin metal of 5~10nm of thermal evaporation deposition on the seed layer again, so as to which ultrathin metal electrode be prepared.Under same thickness, the ultrathin electrodes that the method for the present invention is deposited faster form a film, and defect is less, and optical characteristics and electrology characteristic are more preferable.
Description
Technical field
The invention belongs to optoelectronic device technology fields, and in particular to a kind of to be initially formed seed using molecular-layer deposition technology
Layer, and then the method for hydatogenesis ultrathin metal electrode.
Background technology
The transparent electrode generally use indium tin oxide (Indium Tin Oxide, ITO) of organic electronic device at present, but
Since indium is in the shortage of nature, ITO is poor as the mechanical performance of flexible device in itself.Ultrathin metal electrode raw material are certainly
Right boundary derives from a wealth of sources, and with good flexibility, and the materials such as metal gold, silver, copper have excellent flexibility and highly conductive
Property (gold：2.35μΩcm；Silver：1.59μΩcm；Copper：1.67 μ Ω cm) feature, work function is between 4.6ev and 5.1ev, easily
Be conducive to carrier injection in forming Ohmic contact with p/n doped organic layers, be suitable as opto-electronic device electrode.Therefore, just
Gradually substitution ITO, becomes the hot spot studied at present.However metal has very high extinction coefficient, metallic film is transparent to realize
Change, while weaken the microcavity effect that metal electrode is formed as far as possible, the thickness of the super thin metal film of Grown generally should
Less than 10nm.But the surface energy differential of super thin metal and substrate is different larger during due to hydatogenesis, is not easy to form effective attachment, cause
Quality of forming film is poor, and conductivity becomes smaller.At present, can metal electrode and substrate be improved by the method for Seed Layer (seed layer)
Between surface attachment, improve quality of forming film.
Thin film deposition has two kinds of forms of chemisorbed and physical absorption, during physical absorption, substrate and the atom close to surface
Or molecule is only adsorbed with the electrostatic interaction of Van der Waals for, electric dipole, electric quadrupole etc..This depositional mode
Adsorption capacity is small, and easily forms island growth, and island structure can generate displacement during growth, causes growth uneven,
Therefore there are a large amount of defects.Chemisorbed can successively (layer by layer, LBL) be grown, substrate with close to table
The atom or molecule in face combine (electron covalent bond, ionic bond, atom key, metallic bond etc.) in the form of constitutional chemistry key；It is this
Depositional mode adsorption capacity is big, and tuberculosis point is more during growth, it is intended to LBL layer growths, the ultrathin metal electrode grown
Better quality.Such as Bi, Yan-Gang etc. (Nanoscale, 2016,8,10010-10015) growth is used for the ultra-thin gold of OLED
Anode, SU-8 interact to fix metallic atom to inhibit island by the chemical bond between Au and SU-8 films as Seed Layer
Growth pattern.SU-8 enhances the chemical adsorption capacity of substrate and ultra-thin metal layer as Seed Layer, in research before Cu,
ZnO, Co, Ni are also once used for Seed Layer.
Molecular-layer deposition (Molecular layer deposition, MLD) is a kind of advanced organic polymer with having
Machine inorganic hybrid film technology of preparing generates films by two kinds of presoma alternation responses, and when growth can be accurately controlled cycle
Number is to form a kind of self-limiting growth method of deposition film based on Chemisorption.By gas phase forerunner in MLD deposition process
Body pulse is alternately passed through reactor, and precursor reaches substrate surface, they in its chemical absorption of surface and can react,
The reactant for participating in reaction every time is confined to chemisorbed in the molecule of substrate surface, due to a large amount of chemical bond of Surface Creation,
Be allowed to all generate strong bonding action (bonding effect) between transparent substrates and metallic molecule, with inhibit metal and
Substrate interface is layered, it is therefore believed that MLD technologies can be utilized to form super thin metal Seed Layer, is easier chemisorbed
It is formed, promotes super thin metal growth.
Invention content
The object of the present invention is to provide a kind of methods of depositing high-quality ultrathin metal electrode, are specifically to utilize molecular layer
Deposition method (MLD) grows Seed Layer, carries out ultrathin electrodes growth, the increased chemisorbed of MLD Seed Layers on the seed layer
Make ultrathin electrodes that there is better photoelectric characteristic under same thickness.
The method of the present invention that ultrathin metal electrode is prepared based on molecular-layer deposition technology, its step are as follows：
1) reaction chamber of molecular-layer deposition equipment is placed the substrate into, be heated to 100~300 DEG C and keeps stable；It vacuumizes
After be passed through carrier gas (nitrogen, argon gas etc.), make cavity stable gas pressure in 0.1~0.3Torr；
2) deposited seed layer：0.02~20s presomas 1 are passed through into reaction chamber, are allowed to and substrate surface chemical bonding reaction
Half product is generated, 5~150s carrier gas is passed through and discharges extra presoma 1 and by-product；It is passed through 0.02~20s presomas 2 again, makes
Reacted with half product, substrate surface generation layer of surface carry original chemical key molecular layer, be passed through 5~150s carrier gas will
Extra presoma 2 is discharged with by-product；It is passed through presoma 1 more than repeating, is passed through carrier gas, being passed through presoma 2, the step for being passed through carrier gas
It is rapid repeatedly, so as to obtain the Seed Layer that the surface that thickness is 10~100nm has a large amount of regular chemical bonds in substrate surface；
3) step 2) growth Seed Layer on 5~10nm of thermal evaporation deposition super thin metal, it is ultra-thin so as to be prepared
Metal electrode.
The above method step 1) substrate includes being not limited to silicon chip, glass, silica, PI (polyimides), PET
(polyethylene terephthalate), PEN (polyethylene naphthalate), sapphire etc..
The above method step 2) Seed Layer includes being not limited to polyamide (binary acid+diamine), polyester-imide (four
First acid+diamine) etc. the organic inorganic hybridizations object such as organic polymers or metal oxygen alkane (organometallic alkyl compound+dihydric alcohol).
The above method step 3) super thin metal includes being not limited to silver, copper, gold, aluminium, titanium, palladium etc..
It is the effective of solution super thin metal film growth using " Seed Layer " that MLD technologies are formed between metal and substrate
Means.Molecule organic layer can be by changing its end moieties come the physicochemical properties of accurate control surface, so its energy
It is enough used to change and control substrate surface reactions.With MLD deposited seed layers, chemistry suction between substrate and metallic atom is enhanced
The attached super thin metal for making growth is inclined to layer growth.Under same thickness, ultrathin electrodes that this method is deposited faster into
Film, defect is less, and optical characteristics and electrology characteristic are more preferable.
Description of the drawings
Fig. 1：Super thin metal Direct precipitation (a) prepares metal electrode schematic diagram with adding in seed layer deposition (b)；It is wherein most lower
Layer is glass, and middle layer is MLD Seed Layer aikyiaiurnirsoxan betas, and top layer is gold electrode.
Fig. 2：Atomic force microscopy of the aikyiaiurnirsoxan beta as the ultra-thin gold electrode of seed layer deposition in glass substrate.Wherein exist
The gold (a) of 3nm is grown in substrate of glass；Grow the aikyiaiurnirsoxan beta regrowth 3nm's of about 20n m with MLD methods on the glass substrate
Golden (b)；The gold (c) of the aikyiaiurnirsoxan beta regrowth 5nm of about 20nm is grown with MLD methods on the glass substrate；It uses on the glass substrate
The gold (d) of the aikyiaiurnirsoxan beta regrowth 7nm of MLD methods growth about 20nm；
Fig. 3：The organic luminescent device voltage that ITO electrode is prepared with the ultra-thin gold electrode grown using the method for the present invention-bright
Spend characteristic curve (a) and voltage-to-current efficiency curve (b).
Specific embodiment
The present invention is specifically described in the following with reference to the drawings and specific embodiments.
Embodiment 1
Glass substrate after ultrasonic cleaning is put into the reaction of molecular-layer deposition equipment (Jiaxing section people, PEALD-150A)
Chamber is heated to 120 DEG C and keeps stable；Nitrogen is passed through after vacuumizing, nitrogen flow 20sccm makes cavity stable gas pressure exist
0.15Torr；
Presoma 1 is trimethyl aluminium, and presoma 2 is ethylene glycol, and carrier gas is nitrogen, and t1, t2, t3, t4 are respectively trimethyl
Aluminium be passed through the burst length (0.04s), scavenging period (60s), ethylene glycol are passed through burst length (0.4s), scavenging period
(120s).T1-t4 is respectively 0.04s, 60s, 0.4s, 120s.Trimethyl aluminium does not heat, and the heating temperature of ethylene glycol is 80 DEG C
(trimethyl aluminium and these presomas of ethylene glycol containment portion, can be with independent heating).It is recycled for totally 200, obtained using MLD depositions
To the thickness about 20nm of aikyiaiurnirsoxan beta Seed Layer.
Secondly in the substrate of glass with aikyiaiurnirsoxan beta Seed Layer with 3 angstroms of per second speed thermal evaporations growth thickness 3nm, 5nm,
The super thin metal of 7nm is golden (Au), obtains having the substrate of glass based on MLD Seed Layer super thin metals；In addition again in another piece of glass
One group of contrast experiment is in glass substrate --- only the super thin metal of growth 3nm is golden (Au) on the glass substrate.As schemed (b) AFM tables
Shown in the aspect graph of face, the similary gold for depositing 3nm, the Au in aikyiaiurnirsoxan beta Seed Layer is evenly inclined to film forming.In aikyiaiurnirsoxan beta Seed Layer
The Au of 5nm has formed a film, and film forming is uniform during 7nm, i.e., super thin metal thickness can be made to be reduced to 5 using MLD aikyiaiurnirsoxan betas as Seed Layer
~7nm.
Embodiment 2
The method of preparation aikyiaiurnirsoxan beta in embodiment 1 is constant, uses four dimethyl amine zirconiums (presoma 1, heating 70
DEG C) and ethylene glycol (presoma 2, heat 80 DEG C) prepare zirconium oxygen alkane (t1=0.06, t2=120s, t3=0.4s, t4=120s)
As Seed Layer.
Two kinds of following OLED device of thermal evaporation organic film plating equipment preparation structure are utilized on this basis：
Glass/zirconium oxygen alkane (20nm)/gold (7nm)/HAT (5nm)/TAPC (45nm)/CBP (Irppy3 mass doping 10%)
20nm/TPBi(50nm)/LiF(0.8nm)/Al(100nm)；
Glass/ITO/HAT (5nm)/TAPC (45nm)/CBP (Irppy3 mass doping 10%) 20nm/TPBi (50nm)/
LiF(0.8nm)/Al(100nm)。
Wherein Au and ITO be anode, HAT (C18N12, No. CAS：It is 105598-27-4) hole injection layer, TAPC
(C46H46N2, No. CAS：It is 58473-78-2) hole transmission layer, CBP (C36H24N2, No. CAS：58328-31-7) and Ir (ppy) 3
(C33H24IrN3, No. CAS：It is 94928-86-6) doping luminescent layer, TPBi (C45H30N6, No. CAS：192198-85-9) it is electronics
Transport layer, LiF are electron injecting layer, and Al is cathode, and all material all can be directly commercially available.As a result 1 as shown in figure 3, be based on
This method prepares the OLED device of gold electrode than traditional ITO device efficiencies higher, and 8V is identical with first two device brightness.
Claims (5)
1. a kind of method that ultrathin metal electrode is prepared based on molecular-layer deposition technology, its step are as follows：
1) reaction chamber of molecular-layer deposition equipment is placed the substrate into, be heated to 100~300 DEG C and keeps stable；Lead to after vacuumizing
Enter carrier gas, make cavity stable gas pressure in 0.1~0.3Torr；
2) deposited seed layer：0.02~20s presomas 1 are passed through into reaction chamber, are allowed to generate with substrate surface chemical bonding reaction
Half product is passed through 5~150s carrier gas and discharges extra presoma 1 and by-product；Be passed through 0.02~20s presomas 2 again, be allowed to
Half product reacts, and carries the molecular layer of original chemical key in substrate surface generation layer of surface, being passed through 5~150s carrier gas will be extra
Presoma 2 is discharged with by-product；Repeat it is above is passed through presoma 1, is passed through carrier gas, be passed through that presoma 2, to be passed through the step of carrier gas more
It is secondary, so as to obtain the Seed Layer that the surface that thickness is 10~100nm has a large amount of regular chemical bonds in substrate surface；
3) step 2) growth Seed Layer on 5~10nm of thermal evaporation deposition super thin metal, so as to which super thin metal be prepared
Electrode.
2. a kind of method that ultrathin metal electrode is prepared based on molecular-layer deposition technology as described in claim 1, feature are existed
In：Substrate described in step 1) is silicon chip, glass, silica, polyimides, polyethylene terephthalate, poly- naphthalenedicarboxylic acid
Glycol ester or sapphire.
3. a kind of method that ultrathin metal electrode is prepared based on molecular-layer deposition technology as described in claim 1, feature are existed
In：Carrier gas described in step 1) is nitrogen or argon gas.
4. a kind of method that ultrathin metal electrode is prepared based on molecular-layer deposition technology as described in claim 1, feature are existed
In：Seed Layer described in step 2) is polyamide, polyester-imide or metal oxygen alkane.
5. a kind of method that ultrathin metal electrode is prepared based on molecular-layer deposition technology as described in claim 1, feature are existed
In：Super thin metal described in step 3) is silver, copper, gold, aluminium, titanium or palladium.
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Cited By (2)
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| CN111560601A (en) * | 2019-02-13 | 2020-08-21 | 东京毅力科创株式会社 | Substrate processing method and substrate processing apparatus |
| WO2021114347A1 (en) * | 2019-12-10 | 2021-06-17 | Tcl华星光电技术有限公司 | Method for preparing metal electrode |
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Application publication date: 20180706 |