CN100593871C - Organic field-effect transistors having high mobility and preparation thereof - Google Patents
Organic field-effect transistors having high mobility and preparation thereof Download PDFInfo
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- CN100593871C CN100593871C CN200810118129A CN200810118129A CN100593871C CN 100593871 C CN100593871 C CN 100593871C CN 200810118129 A CN200810118129 A CN 200810118129A CN 200810118129 A CN200810118129 A CN 200810118129A CN 100593871 C CN100593871 C CN 100593871C
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Abstract
The invention discloses an organic field effect transistor and a preparation method thereof. The organic field effect transistor comprises a substrate, a gate electrode positioned on the substrate, aninsulating layer positioned on the gate electrode, a blending layer which is made from a polymer and dipole molecules and is positioned on the insulating layer, an organic semiconductor layer which is positioned on the blending layer of the polymer and the dipole molecules, and a source electrode and a drain electrode which are positioned on the organic semiconductor layer. The organic field effect transistor of the invention controls the property of a conducting channel by controlling the dipole moment of the dipole molecules in a polymer-dipole molecule decorated layer, and can adjust and control the mobility of the organic field effect transistor, and can randomly change the composition of the polymer-dipole molecule decorated layer and the organic semiconductor layer, which is suitable for constructing a high-mobility field effect transistor and has application value when preparing high-mobility organic field effect transistors and high-performance organic semiconductor logic gates and integrated circuits.
Description
Technical field
The present invention relates to a kind of organic field effect tube and preparation method thereof with high mobility.
Background technology
(Tsumura since first organic field effect tube report, A., Koezuka, H., Ando, T.Appl.Phys.Lett.49,1210,1986), organic field effect tube is because it is in Active Matrix LCD At, the organic integration circuit, the potential using value of aspects such as electronic trademark has obtained people's extensive concern.Compare with inorganic transistors, it is low, in light weight that organic field effect tube has a cost, and pliability is good, is easy to characteristics such as mass preparation.In recent years, organic field effect tube has been obtained significant progress, and the trial (Nature, 403,521-523,2000) that is applied to integrated circuit has been arranged.But generally speaking, the mobility of organic field effect tube is lower (generally all at 0.1～1cm
2V
-1s
-1), limit them and moved towards the possibility of practical application.
The organic field effect tube of high mobility is the necessary unit that realization is used for the organic integration circuit of Organic Light Emitting Diode display driver.For the Organic Light Emitting Diode display driver, require mobility greater than 1cm
2V
-1s
-1At present, people realize this purpose by several different methods, the hydrophobic chlorosilane unimolecule of current topmost employing long-chain self assembly layer (D.K.Aswal, S.Lenfant, D.Guerin, J.V.Yakhmi, D.Vuillaume, Anal.Chim.Acta 2006,568,84) or polymer-modified (R.Ruiz, D.Choudhary, B.Nickel, T.Toccoli, K.C.Chang, A.C.Mayer, P.Clancy, J.M.Blakely, R.L.Headrick, S.Iannotta, G.G.Malliaras, Chem.Mater.2004,16,4497) insulating barrier, perhaps at higher underlayer temperature deposit molecule organic semiconductor (M.H.Yoon, C.Kim, A.Facchetti, T.J.Marks, J.Am.Chem.Soc.2006,128,12851).The chlorosilane self assembled monolayer that also has the report employing to have strong electron-withdrawing group group is recently modified and is improved interface carrier concentration (K.P.Pernstich, C.Goldmann, C.Krellner, D.Oberhoff, D.J.Gundlach, B.Batlogg, Synth.Met.2004,146,325., S.Kobayashi, T.Nishikawa, T.Takenobu, S.Mori, T.Shimoda, T.Mitani, H.Shimotani, N.Yoshimoto, S.Ogawa, Y.Iwasa, Nat.Mater.2004,3,317).Though these research work all make the interface carrier concentration increase substantially, the drift on a large scale of the threshold voltage of device, the on-off ratio (K.P.Pernstich that sharply descends, S.Haas, D.Oberhoff, C.Goldmann, D.J.Gundlach, B.Batlogg, A.N.Rashid, G.Schitter, J.Appl.Phys.2004,96,6431).This class device mostly is to be transformed into the depletion type mode of operation from enhancement mode, for totally unfavorable to the application of aspects such as the exigent Organic Light Emitting Diode driving of on-off ratio.
Summary of the invention
The purpose of this invention is to provide a kind of organic field effect tube and preparation method thereof with high mobility.
Organic field effect tube provided by the present invention comprises substrate, is positioned at gate electrode on the described substrate, is positioned at insulating barrier on the described gate electrode, is positioned at the blend layer of being made up of polymer and dipole molecule on the described insulating barrier, is positioned at the organic semiconductor layer on described polymer and the dipole molecule blend layer and is positioned at source electrode and drain electrode on the described organic semiconductor layer.
For the ease of using, can on described substrate, go between described gate electrode and described contact conductor conducting by intercalation electrode.
The method of the above-mentioned organic field effect tube of preparation provided by the present invention may further comprise the steps:
1) on substrate, deposits layer of metal at least, obtain gate electrode;
2) on described gate electrode, adopt the mode of insulating barrier film forming to deposit one deck insulating barrier at least;
3) deposited polymer and dipole molecule blend layer on described insulating barrier;
4) on described blend layer, adopt the organic substance film build method to prepare organic semiconductor layer;
5) preparation source electrode and drain electrode on described organic semiconductor layer obtain organic field effect tube.
Wherein, the described substrate of step 1) is used ethanol, acetone ultrasonic cleaning, deionized water rinsing successively, through nitrogen dry up with oven for drying after plated metal, obtain gate electrode.
Described polymer and dipole molecule blend layer are made of polymer and dipole molecule, and described polymer specifically can be polystyrene (PS), polymethyl methacrylate (PMMA) or Merlon (PC); Described dipole molecule specifically can be urea or dithiooxamide; The thickness of described polymer and dipole molecule blend layer can be 0.5-200nm.Deposition process in the described step 3) is any in following four kinds of methods: vacuum vapour deposition, get rid of embrane method, drip embrane method and print process.
Described organic semiconductor layer is to be made of organic small molecule material and/or macromolecule polymer material; Described organic small molecule material specifically can be pentacene, connects six thiophene, aphthacene or fluorine CuPc; The thickness of described organic semiconductor layer is 20-200nm, can select in 20～200 nanometer range as required, as select 25 nanometers, 50 nanometers or 75 nanometers, or 100 nanometers.The organic substance film build method is a kind of in following four kinds of methods in the described step 4): vacuum vapour deposition, get rid of embrane method, drip embrane method and print process.
The thickness of described source electrode and drain electrode can be 10-300nm; The length of raceway groove can be 0.2-150 μ m between described source electrode and the drain electrode.
The present invention has following characteristics and advantage:
1, the organic field effect tube of the present invention preparation is controlled the character of conducting channel, the mobility of adjustable organic field effect tube by the dipole moment size of dipole molecule in control polymer-dipolar molecule-modified layer;
2, method disclosed by the invention is compared with other method, can utilize same prepared to obtain performance and strengthen the organic field effect tube of device parameters narrow distribution;
3, method disclosed by the invention, can change the composition of polymer-dipolar molecule-modified layer and organic semiconductor layer arbitrarily, be easy to construct high-mobility field-effect transistor, in the preparation of the organic effect transistor of high mobility and high-performance organic semiconductor gate and integrated circuit, using value arranged;
4, organic field effect tube of the present invention all has universality to different organic semiconductors, and this performance for miscellaneous molecule organic semiconductor provides a kind of new way.
Description of drawings
Fig. 1 is the structural formula of polymer molecule in the embodiment of the invention, dipole molecule and organic semiconducting materials molecule; Wherein, A1-A3 is a polymer molecule, A1-polystyrene, A2-polymethyl methacrylate, A3-Merlon; B1-B2 is a dipole molecule, and B1 is a urea, and B2 is a dithiooxamide; C1-C2 is the organic semiconducting materials molecule, and C1 is a pentacene, and C2 is for connecting six thiophene;
Fig. 2 is the structural representation of FET device of the present invention, and wherein, 1 is gate electrode, and 2 is insulating barrier, and 3 is polymer-dipolar molecule-modified layer, and 4 is organic semiconductor layer, and 5 is the source electrode, and 6 is drain electrode;
Fig. 3 is the curve of output of organic field effect tube, wherein, Fig. 3 a among the embodiment 1 based on the curve of output of the organic field effect tube for preparing on the silicon dioxide insulating layer (no polymer-dipolar molecule-modified layer), Fig. 3 b is the curve of output of the organic field effect tube (no polymer-dipolar molecule-modified layer) for preparing on the silicon dioxide insulating layer of modifying based on octadecyl chlorosilane (OTS) among the embodiment 1.
Fig. 4 is the curve of output and the transfer curve of organic field effect tube; Wherein, Fig. 4 a is the curve of output of the organic field effect tube modified based on polystyrene among the embodiment 1, and Fig. 4 b be the curve of output of the organic field effect tube for preparing of embodiment 1, and Fig. 4 c is four kinds of transistorized transfer curves among the embodiment 1;
Fig. 5 is the curve of output and the transfer curve of organic field effect tube; Wherein, Fig. 5 a is the curve of output of the organic field effect tube modified based on polystyrene among the embodiment 2, and Fig. 5 b be the curve of output of the organic field effect tube for preparing of embodiment 2, and Fig. 5 c is two kinds of transistorized transfer curves among the embodiment 2.
Embodiment
Below in conjunction with accompanying drawing the present invention is described in detail, but the present invention is not limited thereto embodiment.
The structure of organic field effect tube of the present invention is as shown in Figure 2: be followed successively by gate electrode 1, insulating barrier 2, polymer-dipolar molecule-modified layer 3, organic semiconductor layer 4, source electrode 5 and drain electrode 6 from the bottom up.
Technical scheme of the present invention is the extra one layer of polymeric-dipole molecule blend decorative layer that increases between insulating barrier and organic semiconductor layer.The structure of this device comprises substrate, gate electrode 1, insulating barrier 2, polymer-dipolar molecule-modified layer 3, organic semiconductor layer 4, source electrode 5 and drain electrode 6; It constructs insulating barrier 2, polymer-dipolar molecule-modified layer 3, organic semiconductor layer 4, source electrode 5 and drain electrode 6 in turn after deposition and pattern gate electrode 1 on the substrate.
Described substrate is that one of them is made by metal, glass, pottery, polymer, silicon chip.
Described gate electrode 1, source electrode 5 and drain electrode 6, be to constitute by having low-resistance material, comprise various metals and alloy materials such as gold, silver, aluminium, copper, metal oxide (as tin indium oxide) electric conducting material and conducing composite material (as gold size, elargol, carbon paste etc.), deposition process can be various deposition processs such as the chemical vapour deposition (CVD) that strengthens of vacuum thermal evaporation, magnetron sputtering, plasma, silk screen printing, printing, coating.
Described insulating barrier 2 materials have excellent dielectric properties, comprise inorganic insulating material such as silicon dioxide, silicon nitride, aluminium oxide, titanium dioxide, tantalum pentoxide, organic insulating material such as polystyrene, polymethyl methacrylate, polyvinyl alcohol etc., the preparation method can be the chemical vapour deposition (CVD), the thermal oxidation that strengthen of plasma, get rid of film or vacuum evaporation etc.The thickness of described insulating barrier is 100 nanometers～500 nanometers.Can in 100 nanometers～500 nanometer range, select as required, as 100 nanometers, or 200 nanometers, or 300 nanometers, or 400 nanometers, or 500 nanometers.
Described polymer-dipolar molecule-modified layer 3 is between insulating barrier 2 and organic semiconductor layer 4, as the carrier mobility key-course.
Described polymer-dipolar molecule-modified layer 3 is made of polymer and dipole molecule, (dipole moment is greater than the molecule of 1.5 debye for described dipole molecule, be also referred to as strong polar molecule), comprise inorganic molecule, organic molecule, dye molecule, macromolecule and their derivative or their mixture.
Described organic semiconductor 4 adopts the organic material with field effect behavior, comprises organic small molecule material, macromolecule polymer material or their mixtures.
Described organic semiconductor layer 4 adopts individual layer or bilayer, adopts a kind of material or composite material.
The film build method of described polymer-dipolar molecule-modified layer 3 and semiconductor layer 4 is for vacuum evaporation, get rid of film, drip film, printing; When organic substance is polymer, adopts and get rid of film, drip film, printing; During for micromolecule, adopt vacuum evaporation, get rid of film, drip film, impression, printing.
The thickness that described drain electrode 6 and source electrode are 5 layers is 10 nanometers～300 nanometers.Can in 10 nanometers～300 nanometer range, select as required, as 30 nanometers or 100 nanometers or 200 nanometers or 300 nanometers.
0.2 micron～150 microns of described channel lengths.Can in 0.2 micron～150 micrometer ranges, select as required, as 0.2 micron or 50 microns or 100 microns or 150 microns.
A among Fig. 1
1-A
3Shown is is used to prepare the molecular formula of the polymer of organic field effect tube of the present invention, is polystyrene (PS) polymethyl methacrylate (PMMA), Merlon (PC); B among Fig. 1
1-B
2Shown is the molecular formula of dipole molecule urea and dithiooxamide (being the Aldrich commercial prod); C among Fig. 1
1-C
2Be used active semiconductor layer molecule pentacene and the chemical constitution schematic diagram that connects six thiophene.
Shown in Figure 2 be the structural representation of organic field effect tube of the present invention; Wherein: the bottom is a gate electrode 1, and its top is an insulating barrier 2, is respectively polymer-dipolar molecule-modified layer 3 and organic semiconductor layer 4 then; The top is source electrode 5 and drain electrode 6.
Embodiment 1,
Channel length L is 50 microns, and source electrode 5, drain electrode 6 are gold electrode, and silicon dioxide is insulating barrier 2, based on the preparation of the organic field effect tube of the polymer of polystyrene-urea-dipolar molecule-modified layer 3 and pentacene organic semiconductor layer 4.
The preparation method of this organic field effect tube comprises following concrete step:
The preparation of the first step, gate electrode 1
After polycrystalline silicon substrate is ultrasonic through ethanol, acetone successively, deionized water rinsing, nitrogen dried up, oven dry realized heavily doped to form the gate electrode of conduction to substrate with diffusion technology then;
The deposition of second step, insulating barrier 2
The silicon substrate that deposits gate electrode is placed in the chemical gas-phase deposition system of plasma enhancing deposition of silica.The thickness range of the insulating barrier of transistor high mobility of the present invention is that 100 nanometers are to 500 nanometers.The thickness of insulating barrier is 450 nanometers in the present embodiment.
The deposition of the 3rd step, polymer-dipolar molecule-modified layer 3
With polymer (polystyrene, weight average molecular weight 280,000) and the mixed solution 0.1ml of dipole molecule (urea) (the quality percentage composition of polystyrene be 5% and the molar concentration of urea be 0.01M, the used solvent of mixed solution is a paraxylene), drop on the substrate, start spin coater, polymer-dipole decorative layer will be attached to surface of insulating layer, and the thickness of polymer-dipole decorative layer is 10nm.
The deposition of the 4th step, organic semiconductor layer 4
In vacuum degree is 5 * 10
-4Under the condition of Pa with
Speed deposit pentacene with vacuum deposition method, thickness is 50 nanometers.
The 5th step, the preparation of source electrode 5, drain electrode 6
In vacuum degree is 1 * 10
-3Under the condition of Pa with
Speed by the template gold evaporation, thickness is 50 nanometers, obtains having the gold electrode of interdigital structure.
The 6th step, test
Utilize Keithley 4200SC semi-conductor test instrument that the performance of prepared organic field effect tube is tested.
Fig. 4 b is 50 microns for the channel length of embodiment 1, and source electrode 5, drain electrode 6 are the curve of output of the pentacene organic field effect tube of modifying based on polystyrene-urea of gold electrode.Can clearly find out that device is the field-effect transistor (device presents the field effect regulation and control under negative gate voltage and negative source-drain voltage) of p type from the curve of output.The device of modifying based on polystyrene in Fig. 4 a is compared, and embodiment 1 device current has had significant raising.According to formula I
DS=μ (W/2L) C
i(V
G-V
T)
2, wherein, μ is the mobility of field-effect transistor, W and L are respectively channel width and channel length, C
iBe the electric capacity of insulated gate unit are; Can calculate from Fig. 4 c, the mobility of device is from 0.95 ± 0.13cm
2V
-1s
-1(based on the device of polystyrene modification) brings up to 1.72 ± 0.16cm
2V
-1s
-1(device of modifying based on polystyrene-urea of embodiment 1 preparation), wherein, among Fig. 4 c from top to bottom, above the ordinate of four curve correspondences be | source-drain current | (A), below the ordinate of four curve correspondences be | source-drain current | 1/2 (A) 1/2.This value also is higher than far away at naked silicon chip (Bare) (0.079 ± 0.02cm
2V
-1s
-1) and silicon chip (0.59 ± 0.03cm of modifying of OTS
2V
-1s
-1) go up the mobility of the device that the deposition pentacene obtains.
Embodiment 2,
Method by embodiment 1 prepares organic field effect tube, unique different be pentacene to be replaced to connect six thiophene, be deposited on polymer-dipolar molecule-modified layer 3, the device of this structure also presents the feature that mobility improves.
Fig. 5 b is 50 microns for the channel length of embodiment 2, and source electrode 5, drain electrode 6 are the curve of output of company's six thiophene organic field effect tubes of modifying based on polystyrene-urea of gold electrode.From curve of output, can find out clearly that device is the field-effect transistor of p type, compare that electric current has had significant raising with the device based on polystyrene among Fig. 5 a.Can calculate from Fig. 5 c, the mobility of device is from 0.042 ± 0.003cm
2V
-1s
-1(based on the device of polystyrene modification) brings up to 0.17 ± 0.01cm
2V
-1s
-1(devices of modifying based on polystyrene-urea of embodiment 2 preparation), wherein, among Fig. 5 c from top to bottom, above the ordinate of two curve correspondences be | source-drain current | (A), below the ordinate of two curve correspondences be | source-drain current |
1/2(A)
1/2
Embodiment 3,
Method by embodiment 1 prepares organic field effect tube, unique different be that organic semiconductor layer 4 is aphthacene, be the organic field effect tube of modifying semiconductor layer 3 preparation with polystyrene-urea, mobility is from 0.031 ± 0.005cm
2V
-1s
-1(based on the device of polystyrene modification) brings up to 0.09 ± 0.02cm
2V
-1s
-1
Embodiment 4,
Method by embodiment 1 prepares organic field effect tube, unique different be that organic semiconductor layer 4 is fluorine CuPc F
16CuPc is the organic field effect tube of modifying semiconductor layer 3 preparation with polystyrene-urea, and the mobility of device is from (6 ± 0.7) * 10
-4Cm
2V
-1s
-1(based on the device of polystyrene modification) brings up to (9 ± 0.6) * 10
-3Cm
2V
-1s
-1
Embodiment 5,
Method by embodiment 1 prepares organic field effect tube, unique different be that the urea molecule in polymer-dipolar molecule-modified layer 3 is replaced to the dipole molecule dithiooxamide, the mobility of device is from 0.95+0.13cm
2V
-1s
-1(based on the device of polystyrene modification) brings up to 1.46 ± 0.05cm
2V
-1s
-1
Embodiment 6,
Method by embodiment 1 prepares organic field effect tube, and unique difference replaces to polymethyl methacrylate (weight average molecular weight 320,000) with the polystyrene in polymer-dipolar molecule-modified layer 3, and organic semiconductor layer 4 remains pentacene.The mobility of device is from 0.48 ± 0.06cm
2V
-1s
-1(based on the device of polymethyl methacrylate modification) brings up to 0.76 ± 0.08cm
2V
-1s
-1
Method by embodiment 1 prepares organic field effect tube, and unique difference replaces to Merlon (weight average molecular weight 540,000) with the polystyrene in polymer-dipolar molecule-modified layer 3, and organic semiconductor layer 4 remains pentacene.The mobility of device is from 0.55 ± 0.02cm
2V
-1s
-1(based on the device of Merlon modification) brings up to 1.17 ± 0.15cm
2V
-1s
-1
Describing above is to be used to realize the present invention and embodiment, and those of ordinary skills can determine multiple implementation according to actual conditions, and therefore, scope of the present invention should not described by this and limit.It should be appreciated by those skilled in the art,, all belong to claim of the present invention and come restricted portion in any modification or partial replacement that does not depart from the scope of the present invention.
Claims (10)
1, a kind of organic field effect tube comprises substrate, is positioned at gate electrode on the described substrate, is positioned at insulating barrier on the described gate electrode, is positioned at the blend layer of being made up of polymer and dipole molecule on the described insulating barrier, is positioned at the organic semiconductor layer on described polymer and the dipole molecule blend layer and is positioned at source electrode and drain electrode on the described organic semiconductor layer;
Described polymer is polystyrene, polymethyl methacrylate or Merlon; Described dipole molecule is urea or dithiooxamide.
2, organic field effect tube according to claim 1 is characterized in that: the thickness of the described blend layer of being made up of polymer and dipole molecule is 0.5-200nm.
3, organic field effect tube according to claim 1 is characterized in that: described organic semiconductor layer is to be made of organic small molecule material and/or macromolecule polymer material; The thickness of described organic semiconductor layer is 20-200nm.
4, field-effect transistor according to claim 3 is characterized in that: described organic small molecule material is pentacene, company six thiophene, aphthacene or fluorine CuPc.
5, organic field effect tube according to claim 1 is characterized in that: the thickness of described source electrode and drain electrode is 10-300nm; Channel length between described source electrode and the drain electrode is 0.2-150 μ m.
6, a kind of method for preparing arbitrary described organic field effect tube among the claim 1-5 may further comprise the steps:
1) on substrate, deposits layer of metal at least, obtain gate electrode;
2) on described gate electrode, adopt the mode of insulating barrier film forming to deposit one deck insulating barrier at least;
3) deposited polymer and dipole molecule blend layer on described insulating barrier;
Described polymer and dipole molecule blend layer are made of polymer and dipole molecule, and described polymer is polystyrene, polymethyl methacrylate or Merlon; Described dipole molecule is urea or dithiooxamide;
4) on described blend layer, adopt the organic substance film build method to prepare organic semiconductor layer;
5) preparation source electrode and drain electrode on described organic semiconductor layer obtain organic field effect tube.
7, method according to claim 6 is characterized in that: the described substrate of step 1) is used ethanol, acetone ultrasonic cleaning, deionized water rinsing successively, through nitrogen dry up with oven for drying after plated metal, obtain gate electrode.
8, method according to claim 6 is characterized in that: the described deposition process of step 3) is any in following four kinds of methods: vacuum vapour deposition, get rid of embrane method, drip embrane method and print process; The thickness of described polymer and dipole molecule blend layer is 0.5-200nm.
9, method according to claim 6 is characterized in that: described organic semiconductor layer is to be made of organic small molecule material and/or macromolecular material; Described organic small molecule material is pentacene, company six thiophene, aphthacene or fluorine CuPc; The described organic substance film build method of step 4) is a kind of in following four kinds of methods: vacuum vapour deposition, get rid of embrane method, drip embrane method and print process; The thickness of described organic semiconductor layer is 20-200nm.
10, method according to claim 6 is characterized in that: the thickness of described source electrode and drain electrode is 10-300nm; The length of raceway groove is 0.2-150 μ m between described source electrode and the drain electrode.
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| CN102110776B (en) * | 2010-12-03 | 2012-10-03 | 中国科学院化学研究所 | High-performance Organic field effect transistor and preparation method thereof |
| CN102723436A (en) * | 2011-03-29 | 2012-10-10 | 中国科学院微电子研究所 | Ferroelectric type memory cell, memory and preparation method thereof |
| CN102255046B (en) * | 2011-05-25 | 2013-04-10 | 中国科学院化学研究所 | Transparent organic polymer insulating layer, preparation method thereof and application thereof to organic field effect transistor |
| CN102610757A (en) * | 2012-04-10 | 2012-07-25 | 中国科学院苏州纳米技术与纳米仿生研究所 | Preparation method of organic thin-film field effect transistor |
| CN105006527A (en) * | 2015-06-16 | 2015-10-28 | 南京邮电大学 | High-brightness multicolored organic light-emitting field-effect transistor and preparation method thereof |
| CN105679940A (en) * | 2016-04-19 | 2016-06-15 | 中国科学院化学研究所 | Bipolar polymer field effect transistor and preparation method and application thereof |
| CN106876585A (en) * | 2017-01-19 | 2017-06-20 | 南京邮电大学 | A kind of method that organic field effect tube mobility is improved by short annealing |
| CN110112073B (en) * | 2019-04-22 | 2021-09-24 | 中国科学院微电子研究所 | Preparation method of field effect transistor and field effect transistor |
| CN116546824A (en) * | 2022-05-07 | 2023-08-04 | 浙江大学 | Organic field effect transistor and preparation method thereof |
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