CN100445422C - Organic zinc source for preparing zinc oxide thin film and its preparing method - Google Patents

Organic zinc source for preparing zinc oxide thin film and its preparing method Download PDF

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CN100445422C
CN100445422C CNB2006100205327A CN200610020532A CN100445422C CN 100445422 C CN100445422 C CN 100445422C CN B2006100205327 A CNB2006100205327 A CN B2006100205327A CN 200610020532 A CN200610020532 A CN 200610020532A CN 100445422 C CN100445422 C CN 100445422C
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organic zinc
zinc
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zinc source
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CN1821439A (en
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戴丽萍
邓宏
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University of Electronic Science and Technology of China
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Abstract

The present invention relates to an organic zinc source for preparing zinc oxide thin films and a preparing method for the organic zinc source, which belongs to the field of chemical material synthesizing technology. The major constituent of the organic zinc source is an organic compound belonging to the class of zinc acetate, Zn4 (OH) 2 (O2CCH3) 6.2H2O, and can contain a small amount of ZnO, wherein the organic compound Zn4 (OH) 2 (O2CCH3) 6.2H2O contains a tetrahedral radical Zn4O, hydrogen bonds are formed on a central oxygen atom, four zinc atoms are coordinate with the oxygen atom in a water molecule and are respectively bonded with one of the oxygen atoms in three acetic acid radicals at the same time in order to form a cage compound in macroscopic view, products of thermal decomposition are ZnO, CH4 and CO2. The preparing method for the organic zinc source uses zinc oxide and glacial acetic acid as reactants and uses absolute alcohol as solvent to prepare the organic zinc source through distillation reflux reaction. The organic zinc source of the present invention has the advantages of nontoxicity, low preparing cost, no poison toxic substance generation during decomposition, low decomposition temperature and full adaptation to all requirements of preparing zinc oxide thin films by SSCVD technology, and is especially suitable for the SSCVD technology to prepare zinc oxide thin films. The preparing method of the organic zinc source has the advantages of low prices of required reactants and simple and easily-controlled preparing process.

Description

A kind of organic zinc source of preparing zinc-oxide film and preparation method thereof that is used to
Technical field
A kind of organic zinc source of preparing zinc-oxide film and preparation method thereof that is used to, belong to field of chemical material synthesizing technology, relate to a kind of SSCVD of being used for (single source chemical vapour deposition, promptly single source chemical vapor deposition) technology and prepare organic zinc source of zinc-oxide film and preparation method thereof.
Technical background
ZnO is an a kind of II-VI family wide bandgap compound semiconductor material, has close lattice parameter and energy gap with GaN, and with respect to GaN, and ZnO has higher fusing point and exciton bind energy and good dynamo-electric contingency and lower electronics and induces defective.These excellent specific properties that ZnO film has make it have a wide range of applications at aspects such as surface acoustic wave, solar cell, ultraviolet detector, LED and LD, so ZnO film becomes the focus of current semiconductor material research.
Researched and developed at present the growing technology of many ZnO films, magnetron sputtering, sol-gel method, chemical bath deposition, molecular beam epitaxy, ion beam assisted depositing, film oxidation method, pulsed laser deposition, Metalorganic Chemical Vapor Deposition (MOCVD) etc. have wherein been arranged.And wherein MOCVD is particularly a kind of effective means of monocrystal thin films of preparation zinc-oxide film, generally with zinc ethyl (DEZ) and oxygen or water or other organism as reaction gas, gas phase ZnO molecule formation of deposits ZnO film on substrate that reaction generates under certain temperature and pressure condition.Though this method has obtained certain achievement aspect growing ZnO thin-film, but because the zinc source that this method is generally used is the compound of zinc alkyl(s), this compound can decompose the inflammable and explosive toxic gas of generation in preparation ZnO film process, and characteristics such as that this oxide compound itself has is poisonous, explosive, cost an arm and a leg make that utilizing the MOCVD technology to produce ZnO film low-costly and in high volume is difficult to realize.Therefore seeking a kind of easy to control, nontoxic, cheap zinc source becomes the key of dealing with problems.
SS CVD technology prepares film owing to use the thermolysis of single solid phase source to produce film forming all chemical ingredientss, do not need to add other material in the reaction process, and reaction conditions is comparatively loose, be easy to control, equipment requirements is not high, therefore have other method do not possess or incomparable characteristic, thereby become hot research in recent years.Especially utilizing SS CVD technology to prepare on the ZnO film, people have obtained certain achievement.The single solid phase organic zinc source that a kind of suitable SSCVD technology prepares zinc-oxide film must possess following characteristic:
1〉single solid phase organic zinc source molecular cell must possess film forming all chemical ingredientss;
2〉intermolecular interaction can overcome its volatility at least;
3〉can necessarily lower temperature (200～300 ℃) down the vaporization of fusing back reach on the substrate of heating fully that scission of link decomposes;
4〉decomposes the back and has only pure zinc oxide, and the ratio of Zn: O is 1: 1 that remaining degradation production is a gas at on-chip remaining solid thing;
5〉sedimentary zinc-oxide film has good crystalline orientation on substrate, meets the requirement of device application.
Document was once reported use Zn 4O (CO 2NEt 2) 6As single solid phase organic zinc source, its preparation method is roughly as follows: use ZnEt 2And HNEt 2Be raw material, temperature of reaction will be strict controlled in (because ZnEt below-20 degrees centigrade 2And HNEt 2Inflammable and explosive), feed the CO of suitable flow in the product that generates 2After make solvent with ether again, after logical equimolar steam stirs in the solution more at last Zn 4O (CO 2NEt 2) 6This preparation method's severe reaction conditions, reactions steps is numerous and diverse, and reactant costs an arm and a leg, and is not suitable for suitability for industrialized production.
Summary of the invention
The invention provides a kind of organic zinc source of preparing zinc-oxide film and preparation method thereof that is used to, this organic zinc source is with low cost and nontoxic, can satisfy prerequisite five characteristics of single solid phase organic zinc source that above-mentioned suitable SSCVD technology prepares zinc-oxide film, be very suitable for the suitability for industrialized production of ZnO film; Simple, the easily control of its preparation method, cheap, the nontoxic pollution-free of raw materials cost.
Detailed technology scheme of the present invention is:
A kind of organic zinc source that is used to prepare zinc-oxide film is characterized in that, this organic zinc source is the pulverulent solids mixture, can contain a spot of ZnO, and its main component is that a kind of molecular formula is Zn 4(OH) 2(O 2CCH 3) 62H 2Organic zinc acetate compounds of O.
Described molecular formula is Zn 4(OH) 2(O 2CCH 3) 62H 2Organic zinc acetate compounds of O, its molecular structure comprises a tetrahedral Zn 4O group, and the central oxygen atom has hydrogen bond to form, the oxygen atom ligand in 4 zinc atoms and the water molecules and simultaneously respectively with three acetate moietys in one of them Sauerstoffatom bonding, formation cage compound (as shown in Figure 2) on the macroscopic view.
Described molecular formula is Zn 4(OH) 2(O 2CCH 3) 62H 2Organic zinc acetate compounds product when thermolysis of O is ZnO, CH 4And CO 2, its thermolysis equation is: Zn 4(OH) 2(O 2CCH 3) 62H 2O=4ZnO+6CH 4↑+6CO 2↑.
A kind of preparation method who is used to prepare the organic zinc source of zinc-oxide film as shown in Figure 3, is characterized in that, as reactant, as the reaction upholder that reaction environment is provided, reaction generates Zn with dehydrated alcohol with zinc oxide and glacial acetic acid for it 4(OH) 2(O 2CCH 3) 62H 2O specifically may further comprise the steps:
1, dry reagent contained within: zinc oxide is carried out drying remove after the water treatment stand-byly, glacial acetic acid distilled to handle the back stand-by;
2, dry solvent (reaction upholder): dehydrated alcohol distilled to handle the back stand-by;
3, reaction: the mole proportioning by 2: 3 is got an amount of zinc oxide and glacial acetic acid, and zinc oxide and glacial acetic acid are added fully reaction in the dehydrated alcohol, and its reaction equation is: 4ZnO+6CH 3COOH=Zn 4(OH) 2(O 2CCH 3) 62H 2O;
4, vacuum-evaporation drying: with step 3 fully reacted solution in a vacuum after the evaporation drying gained solids be described a kind of organic zinc source that is used to prepare zinc-oxide film of the present invention.
In the dry reagent contained within process of described step 1, can use baking oven that zinc oxide is carried out drying and remove water treatment, can use anhydrous cupric sulfate that glacial acetic acid is distilled processing.
In the dry reaction upholder process of described step 2, can use Calcium Chloride Powder Anhydrous that dehydrated alcohol is distilled processing.
In the reaction process of described step 3, reaction soln should be heated to the boiling point of dehydrated alcohol, take the reactive mode of distillation and reflux, to accelerate reaction process, to shorten the reaction times; And add anhydrous cupric sulfate on the prolong top and make siccative, with the condensing reflux dehydrated alcohol.
Some explanation about technical solution of the present invention:
One, about the preparation method's of organic zinc source of the present invention explanation:
1, water is to the influence of entire reaction.
Institute of the present invention synthetic is used to prepare the organic zinc source of zinc-oxide film, and entire reaction course all is to carry out under anhydrous condition, and purpose is to promote four Zn atoms and same O Atomic coordinate to form tetrahedral Zn 4The O group, if react in the aqueous solution, reaction generates Zn (O thereby glacial acetic acid then is ionized the formation ion 2CCH 3) 2, and Zn (O 2CCH 3) 2Zn is not equal to 1 with the stoichiometric coefficient ratio of O in the product that decomposes, therefore can cause the ZnO film anoxic of preparation, perhaps need in the process of preparation ZnO film, introduce oxygen source, so just can not get a desired effect and maybe can not use this SSCVD technology simple to operation.The water molecules that generates in the reaction process is non-solvation, just plays a part coordinating group.
2, the reaction times is to the influence of entire reaction.
Because entire reaction carries out in the environment of non-water, so the degree of ionization of acetate seldom, so speed of response very slow (reaction times is about 48 hours), causes the reaction times very long, and the growth in reaction times can make the abundant coordination of reacted water molecules.
3, dehydrated alcohol is to the influence of entire reaction.
In the entire reaction course, dehydrated alcohol itself is not participated in reaction, only provides the environment of a reaction, and the contact probability of reaction energy and raising reactant promptly is provided.The variation of dehydrated alcohol no quality and quantity before and after reaction, therefore can reclaim purification ethanol in suitability for industrialized production makes it recycle, to save capital.
4, use the explanation of vacuum-evaporation exsiccant.
Owing to dehydrated alcohol is inflammable and explosive organism, in thermostat container, heat to set off an explosion easily the therefore suitable method of selecting the vacuum decompression desciccate for use.
Two, about the explanation of organic zinc source of the present invention:
1, the parsing of chemical molecular formula.
By the infrared transmission spectrogram (Fig. 2) of organic zinc source of the present invention as can be known, this zinc source main component is the Zn with tetrahedral structure 4The cage compound of O group, and the central oxygen atom has hydrogen bond to form, the O Atomic coordinate in 4 Zn atoms and the water molecules and simultaneously respectively with three acetate moietys in one of them Sauerstoffatom bonding.Whole molecular formula Zn 4(OH) 2(O 2CCH 3) 62H 2O is a symmetrical structure, designs simplification formula such as accompanying drawing 1.In addition, because entire reaction can not be carried out fully, make in the product inevitably remaining a spot of ZnO, because a spot of ZnO does not influence the quality of forming film that this zinc source is used to prepare ZnO film, so the organic zinc source that is used to prepare zinc-oxide film of the present invention can contain a spot of ZnO, but its main component is Zn 4(OH) 2(O 2CCH 3) 62H 2O.
2, be applied to the explanation that the SSCVD technology prepares zinc-oxide film about organic zinc source of the present invention.
Zn 4(OH) 2(O 2CCH 3) 62H 2O begins to decompose at 211 ℃, decomposition temperature is relatively low, grow on substrate thereby make film easily be in equilibrium state, it is to utilize this zinc source to have lower temperature fusing and vaporization under lower vacuum condition that the SSCVD technology prepares zinc-oxide film, decomposes film forming then on the hot radical sheet.Its thermolysis equation is: Zn 4(OH) 2(O 2CCH 3) 62H 2O=4ZnO+6CH 4↑+6CO 2↑.Begin to decompose at 211 ℃ by this as can be known organic zinc source of thermogravimetric analysis, decompose fastest in the time of 240 ℃, decompose fully in the time of 260 ℃ (Fig. 4), the product that is decomposed by XPS analysis is ZnO, and the stoichiometric coefficient of Zn and O ratio is about 1: 1 in (accompanying drawing 5,6), and XRD analysis has the application requiring (Fig. 7) that good crystalline orientation meets device based on the SSCVD technology with the ZnO film that this source prepares.
The invention has the beneficial effects as follows:
1: organic zinc source of the present invention is nontoxic, and preparation cost is low, and non-poisonous material generation and decomposition temperature are low during decomposition.
2: the required reactant low price of the preparation method of organic zinc source of the present invention, preparation process are simple and easy to control.
3: organic zinc source of the present invention is fit to all requirements that the SSCVD technology prepares zinc-oxide film fully, is particularly useful for the SSCVD technology and prepares zinc-oxide film.
Description of drawings
Fig. 1 is single solid phase organic zinc source chemical structure skeleton symbol, and it is to comprise a tetrahedral Zn 4The cage compound of O group, i.e. four zinc atoms of an oxygen bonding.Wherein each zinc atom more respectively with one of them Sauerstoffatom bondings of three aceticoceptors, the Sauerstoffatom in zinc and the water molecules is stablized coordination, and the central oxygen atom has hydrogen bond to form, the hydrogen atom in the water molecules forms hydrogen bond with wherein oxygen respectively.
Fig. 2 is the infrared spectrum of single solid phase organic zinc source, and wave number is at 3426.0cm -1, 3251.4cm -1, 3174.3cm -1And 2941.0cm -1Be respectively the γ among the Zn-OH (H-O), γ (Zn-OH)And γ (Zn-O-Zn), wave number is 1563.0cm -1～～1414.6cm -1Be the eigen vibration peak of carboxyl, owing to form coordinate bond with Zn, wave number all moves to low.1314.3cm -1Be-the formation vibration peak of OH group, wave number is 1049.1cm -1～447.4cm -1By the stretching vibration and the flexural vibration characteristic peak that are Zn-O and Zn-OH, can know the ratio of each group by inference according to the intensity at its peak, but this infers its chemical molecular formula Zn thus 4(OH) 2(O 2CCH 3) 62H 2O comprises a tetrahedral Zn 4The cage compound of O group, and the central oxygen atom has hydrogen bond to form, the fourier infrared transmission spectrum is analyzed to such an extent that zinc in this precursor and the Sauerstoffatom in the water molecules are stablized coordination, and when thermolysis and the oxygen competitive coordination of acetate moiety group, its structural formula sketch as shown in Figure 1.
Fig. 3 is organic zinc source preparation flow figure of the present invention.
Fig. 4 is the thermogravimetric analysis spectrogram of organic zinc source of the present invention, is begun to decompose at 211 ℃ by this as can be known organic zinc source of thermogravimetric analysis, decomposes fastestly in the time of 240 ℃, decomposes (accompanying drawing 4) in the time of 260 ℃ fully.
Fig. 5 is with the Zn 2p peak of organic zinc source of the present invention based on the XPS analysis collection of illustrative plates of the ZnO film sample of SSCVD technology preparation.
Fig. 6 is with the O1s peak of organic zinc source of the present invention based on the XPS analysis collection of illustrative plates of the ZnO film sample of SSCVD technology preparation.
Among Fig. 6, O 1s peak " 3 " obtains by two Gaussion curves " 1 ", " 2 " match, peak " 1 " is the 1s peak of oxygen in the molecule that film surface absorbs water, and peak " 2 " are the 1s peak of lattice oxygen in the zinc oxide, and these two central points that fit curve lay respectively at 531.78,530.43eV.
Zinc oxygen stoichiometry ratio can be calculated by following formula:
n Zn : n O = S Zn / α Zn S O / α O
Wherein n is the molar content of element; S is an element XPS spectrum peak area; α is the selected sensitivity factor of XPS analysis element.Calculate by analysis, in the film sample zinc oxygen mol ratio very near 1: 1, thereby prove that organic zinc source of the present invention is fit to utilize the SSCVD technology to prepare ZnO film very much.
Fig. 7 is with the XRD analysis collection of illustrative plates of organic zinc source of the present invention based on the ZnO film sample of SSCVD technology preparation.From the XRD diffracting spectrum of sample as can be known, two diffraction peaks of ZnO film are respectively (100) and (101) peaks, and (100) intensity of diffraction peak is much larger than the intensity at (101) peak, thereby proof has good crystalline orientation based on the SSCVD technology with the ZnO film that organic zinc source of the present invention prepares.
Embodiment
Under simple relatively experiment condition, get zinc oxide 0.2mol, glacial acetic acid 0.3mol, be solvent with the about 200ml of dehydrated alcohol; Use baking oven that zinc oxide is carried out drying and remove water treatment, use anhydrous cupric sulfate that glacial acetic acid is distilled processing, use Calcium Chloride Powder Anhydrous that dehydrated alcohol is distilled processing; Then, earlier dehydrated alcohol is placed flask, add zinc oxide and glacial acetic acid again, add the thermal distillation condensing reflux about 48 hours, condensing reflux pipe top is put anhydrous cupric sulfate and is made siccative.Product in the flask of reaction back puts that reduction vaporization is drying to obtain product in the vacuum.The Zn of experiment gained 4(OH) 2(O 2CCH 3) 62H 2Its productive rate of O is 90%.

Claims (5)

1, a kind of organic zinc source that is used to prepare zinc-oxide film is characterized in that, this organic zinc source is the pulverulent solids mixture, contains a spot of ZnO, and its main component is that a kind of molecular formula is Zn 4(OH) 2(O 2CCH 3) 62H 2Organic zinc acetate compounds of O; Described molecular formula is Zn 4(OH) 2(O 2CCH 3) 62H 2Organic zinc acetate compounds of O, its molecular structure comprises a tetrahedral Zn 4O group, and the central oxygen atom has hydrogen bond to form, the oxygen atom ligand in 4 zinc atoms and the water molecules and simultaneously respectively with three acetate moietys in one of them Sauerstoffatom bonding, formation cage compound on the macroscopic view; Described molecular formula is Zn 4(OH) 2(O 2CCH 3) 62H 2Organic zinc acetate compounds product when thermolysis of O is ZnO, CH 4And CO 2, its thermolysis equation is: Zn 4(OH) 2(O 2CCH 3) 62H 2O=4ZnO+6CH 4↑+6CO 2↑.
2, the preparation method of organic zinc source as claimed in claim 1 is characterized in that, as reactant, as the reaction upholder that reaction environment is provided, reaction generates Zn with dehydrated alcohol with zinc oxide and glacial acetic acid for it 4(OH) 2(O 2CCH 3) 62H 2O specifically may further comprise the steps:
1), dry reagent contained within: zinc oxide is carried out drying remove after the water treatment stand-byly, glacial acetic acid distilled to handle the back stand-by;
2), dry reaction upholder: dehydrated alcohol distilled to handle the back stand-by;
3), reaction: the mole proportioning by 2: 3 is got an amount of zinc oxide and glacial acetic acid, and zinc oxide and glacial acetic acid are added fully reaction in the dehydrated alcohol, and its reaction equation is: 4ZnO+6CH 3COOH=Zn 4(OH) 2(O 2CCH 3) 62H 2O;
4), vacuum-evaporation drying: with the abundant reacted solution of step 3) in a vacuum after the evaporation drying gained solids be the described organic zinc source that is used to prepare zinc-oxide film.
3, the preparation method of organic zinc source according to claim 2 is characterized in that, in the dry reagent contained within process of described step 1), uses baking oven that zinc oxide is carried out drying and removes water treatment, uses anhydrous cupric sulfate that glacial acetic acid is distilled processing.
4, the preparation method of organic zinc source according to claim 2 is characterized in that, described step 2) dry reaction upholder process in, use Calcium Chloride Powder Anhydrous that dehydrated alcohol is distilled processing.
5, the preparation method of organic zinc source according to claim 2 is characterized in that, in the reaction process of described step 3), reaction soln is heated to the boiling point of dehydrated alcohol, takes the reactive mode of distillation and reflux, to accelerate reaction process, to shorten the reaction times; And add anhydrous cupric sulfate on the prolong top and make siccative, with the condensing reflux dehydrated alcohol.
CNB2006100205327A 2006-03-21 2006-03-21 Organic zinc source for preparing zinc oxide thin film and its preparing method Expired - Fee Related CN100445422C (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1400331A (en) * 2002-08-07 2003-03-05 浙江大学 Method for growing ZnO film by solid source chemical gas-phase deposition
JP2004099412A (en) * 2002-09-12 2004-04-02 Inst Of Physical & Chemical Res Material having zinc oxide thin film and method for manufacturing the same
US6838308B2 (en) * 2000-08-18 2005-01-04 Tohoku Techno Arch Co., Ltd. Semiconductor polysilicon component and method of manufacture thereof
US6860937B1 (en) * 2000-03-27 2005-03-01 Tohoku Techno Arch Co., Ltd. Method for preparing zinc oxide semi-conductor material

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6860937B1 (en) * 2000-03-27 2005-03-01 Tohoku Techno Arch Co., Ltd. Method for preparing zinc oxide semi-conductor material
US6838308B2 (en) * 2000-08-18 2005-01-04 Tohoku Techno Arch Co., Ltd. Semiconductor polysilicon component and method of manufacture thereof
CN1400331A (en) * 2002-08-07 2003-03-05 浙江大学 Method for growing ZnO film by solid source chemical gas-phase deposition
JP2004099412A (en) * 2002-09-12 2004-04-02 Inst Of Physical & Chemical Res Material having zinc oxide thin film and method for manufacturing the same

Non-Patent Citations (6)

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Title
Microstructure control of ZnO thin films prepared by singlesource chemical vapor deposition. H.Deng a, et al.Thin Solid Films,Vol.458 . 2004
Microstructure control of ZnO thin films prepared by singlesource chemical vapor deposition. H.Deng a, et al.Thin Solid Films,Vol.458 . 2004 *
Single-Source Chemical Vapor Deposition Growth of ZnOThin Films Using Zn4O(CO2NEt2)6. A. J. Petrella, et al.Chem. Mater.,Vol.14 . 2002
Single-Source Chemical Vapor Deposition Growth of ZnOThin Films Using Zn4O(CO2NEt2)6. A. J. Petrella, et al.Chem. Mater.,Vol.14 . 2002 *
Towards new precursors for ZnO thin films bysingle source CVD : the X-ray structures and precursorproperties of zinc ketoacidoximates. Matthew R. Hill , et al.Inorganica Chimica Acta,Vol.358 . 2004
Towards new precursors for ZnO thin films bysingle source CVD : the X-ray structures and precursorproperties of zinc ketoacidoximates. Matthew R. Hill , et al.Inorganica Chimica Acta,Vol.358 . 2004 *

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