CN102602961A - Method for preparing preferentially oriented ammonium chloride thin film - Google Patents
Method for preparing preferentially oriented ammonium chloride thin film Download PDFInfo
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- CN102602961A CN102602961A CN2012100625865A CN201210062586A CN102602961A CN 102602961 A CN102602961 A CN 102602961A CN 2012100625865 A CN2012100625865 A CN 2012100625865A CN 201210062586 A CN201210062586 A CN 201210062586A CN 102602961 A CN102602961 A CN 102602961A
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- thin film
- ammonium chloride
- film
- precursor thin
- preferred orientation
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Abstract
The invention provides a method for preparing a preferentially oriented ammonium chloride thin film, relating to the preparation processes of thin film materials. The method comprises the following steps: firstly washing a silicon chip, then putting metal chlorides into solvents to be dissolved, obtaining a precursor thin film on the silicon chip by a spin coating method and drying the precursor thin film, putting the precursor thin film into a closed container with diamide hydrate, ensuring the precursor thin film sample not to be contacted with diamide, heating the closed container filled with the precursor thin film sample and finally carrying out cooling and drying, thus obtaining the preferentially oriented ammonium chloride thin film. The method has the following beneficial effects: the method dispenses with the conditions of high temperature and high vacuum, has low requirements for apparatuses, is low in production cost and high in production efficiency and is easy to operate; the ammonium chloride thin film grows in the preferential orientation and has better continuity and uniformity; the components and structure of the target product are easy to control by the new process; and the production method which is low in cost and can realize industrialization is provided for preparing the preferentially oriented ammonium chloride thin film.
Description
Technical field
The invention belongs to the preparation technology of thin-film material, relate in particular to a kind of preparation method who on silicon substrate, obtains preferred orientation ammonium chloride film.
Background technology
Thin film technique constantly develops in recent years, and the preparation of various film material with function becomes the focus of research.Usually all need the substrate of supporting film growth when preparing these thin-film materials, for example sheet glass and silicon chip etc., however these substrates generally do not have solubility, and the film of growing above that is difficult for taking off, and is not easy to carry out other researchs or application again.
The object of the invention is for making preferred orientation ammonium chloride film growth, solubility at silicon chip; Then with the silicon chip of ammonium chloride film during as the substrate of other thin-film materials of preparation; Both can make the growth of film preferred orientation; Can be easy to again the ammonium chloride Film Fractionation is fallen, other thin-film material is taken off.
Summary of the invention
The present invention is in order to solve the deficiency of existing film preparing technology, and invented a kind of diverse with preparation method prior art, the preparation technology of ammonium chloride film.
The present invention adopts spin coating-chemical reaction method to prepare the ammonium chloride thin-film material, and the employing silicon chip is a substrate, with metal chloride such as SnCl
22H
2O, CuCl
22H
2O, ZnCl
2, InCl
34H
2O etc. are raw material; Mixtures a kind of or that they are two or more with in deionized water, ethanol, hydrochloric acid, the terepthaloyl moietie are solvent; Earlier prepare certain thickness precursor thin-film with spin-coating method; With the hydrazine hydrate is reductive agent, and heating at a lower temperature makes precursor thin-film generation chemical reaction obtain title product in encloses container.
Concrete preparation method of the present invention comprises the step of following order:
A. carrying out the cleaning of silicon substrate, is that 2mm * 2mm silicon chip is put into trichloromethane by volume with size: the solution of ethanol=5: 1, ultrasonic cleaning 30min; Again silicon substrate is put into acetone: the solution of zero(ppm) water=5: 1, ultrasonic cleaning 30min; In zero(ppm) water, silicon substrate is used ultra-sonic oscillation 30min again; The above-mentioned silicon substrate that obtains is emitted on sends in the glass dish in the baking oven, 100 ℃ down oven dry supply the system film to use.
B. metal chloride is put into solvent, make its dissolving fully.Specifically, can be with 2.0～5.0 parts metal chloride, like SnCl
22H
2O, CuCl
22H
2O, ZnCl
2, InCl
34H
2Wherein one or more such as O are as solute, wherein solvent is that one or more mixture in deionized water, ethanol, terepthaloyl moietie, the hydrochloric acid is a solvent.
C. make the outside evenly substrate of the said solution of application step b, and oven dry, the precursor thin-film sample obtained.Can above-mentioned solution be dripped on the silicon substrate that is placed on the sol evenning machine; Restart sol evenning machine with 200～3500 rev/mins of rotation certain hours; Make on dripping solution coat evenly after, 100 ℃ substrate dried after, repeat once more to drip and dry again after going up aforementioned solution and rotary coating; So repeat 5～15 times, so on silicon substrate, obtained certain thickness precursor thin-film sample.
D. step c gained precursor thin-film sample is placed on the support, but put into the encloses container of hydrazine hydrate, the precursor thin-film sample is not contacted with hydrazine.It is 20～30 parts that hydrazine hydrate is put into, and at a certain temperature, hydrazine can react with muriate, generates ammonium chloride.The above-mentioned encloses container that the precursor thin-film sample is housed is put into baking oven, be heated between 150～200 ℃, soaking time 10～24 hours, cool to room temperature takes out then.
E. with the steps d products therefrom, carry out seasoning after, promptly obtain preferred orientation ammonium chloride film;
The present invention does not need the high temperature high vacuum condition, and low to the plant and instrument requirement, production cost is low, and production efficiency is high, easy handling.The growth of gained ammonium chloride film preferred orientation; And continuity and homogeneity are preferably arranged; The composition and the structure of the easy controlled target product of this novel process, for prepare high performance preferred orientation ammonium chloride film provide a kind of cost low, can realize large-scale industrial production.
Description of drawings
Embodiment
A. the cleaning of silicon substrate: (size is 2mm * 2mm) to clean silicon substrate as previously mentioned.
B. with 2.7 parts of CuCl
22H
2O puts into vial, adds 48.6 parts of ethanol, utilizes more than the ultrasonic vibration 30min, makes the material uniform mixing in the solution.
C. above-mentioned solution is dripped on the silicon substrate that is placed on the sol evenning machine, restart sol evenning machine, sol evenning machine rotated 5 seconds with 200 rev/mins; With 1000 rev/mins of rotations 15 seconds; Make on dripping solution coat evenly after, 100 ℃ substrate dried after, repeat once more to drip and dry again after going up aforementioned solution and rotary coating; So repeat 10 times, so on silicon substrate, obtained certain thickness precursor thin-film sample.
D. the precursor thin-film sample of above-mentioned technology gained is put into sealable container; And put into 24.3 parts of hydrazine hydrates; The precursor thin-film sample places it is not contacted with hydrazine, and the above-mentioned encloses container that the precursor thin-film sample is housed is put into baking oven, is heated to 200 ℃; Soaking time 20 hours, cool to room temperature takes out then.
E. with the steps d products therefrom, carry out seasoning after, promptly obtain preferred orientation ammonium chloride film.
Embodiment 2
A. the cleaning of silicon substrate: (size is 2mm * 2mm) to clean silicon substrate as previously mentioned.
B. with 2.4 parts of CuCl
22H
2O and 1.0 parts of ZnCl
2Put into vial, add 73.2 parts of ethanol, utilize more than the ultrasonic vibration 30min, make the material uniform mixing in the solution.
C. above-mentioned solution is dripped on the silicon substrate that is placed on the sol evenning machine, restart sol evenning machine, sol evenning machine rotated 5 seconds with 200 rev/mins; With 3000 rev/mins of rotations 15 seconds; Make on dripping solution coat evenly after, 100 ℃ substrate dried after, repeat once more to drip and dry again after going up aforementioned solution and rotary coating; So repeat 10 times, so on silicon substrate, obtained certain thickness precursor thin-film sample.
D. the precursor thin-film sample of above-mentioned technology gained is put into sealable container; And put into 24.3 parts of hydrazine hydrates; The precursor thin-film sample places it is not contacted with hydrazine, and the above-mentioned encloses container that the precursor thin-film sample is housed is put into baking oven, is heated to 160 ℃; Soaking time 22 hours, cool to room temperature takes out then.
E. with the steps d products therefrom, carry out seasoning after, promptly obtain preferred orientation ammonium chloride film, its phase composite and the direction of growth are shown in accompanying drawing 1.
Claims (5)
1. the preparation method of a preferred orientation ammonium chloride film comprises the step of following order:
A. the cleaning of silicon substrate;
B. with 2.0～5.0 parts of metal chlorides, put into 30～100 parts solvent, make the material uniform mixing in the solution;
C. make the outside evenly substrate of the said solution of application step b, and oven dry, the precursor thin-film sample obtained;
D. step c gained precursor thin-film sample is placed on the support; But put into the encloses container of hydrazine hydrate; The precursor thin-film sample is not contacted with hydrazine, the encloses container that the precursor film sample is housed is put into baking oven, be heated between 150～200 ℃; Soaking time 10～24 hours, cool to room temperature takes out then;
E. with the steps d products therefrom, carry out seasoning, obtain preferred orientation ammonium chloride film.
2. the preparation method of a kind of preferred orientation ammonium chloride film as claimed in claim 1 is characterized in that, the said cleaning of step a is that silicon substrate size is 2mm * 2mm, puts into trichloromethane by volume: the solution of ethanol=5: 1, ultrasonic cleaning; Again silicon chip is put into acetone: the solution of zero(ppm) water=5: 1, ultrasonic cleaning; In zero(ppm) water, silicon substrate is used ultra-sonic oscillation again; The above-mentioned silicon substrate that obtains is emitted on sends in the baking oven oven dry in the glass dish and supply the system film to use.
3. the preparation method of a kind of preferred orientation ammonium chloride film as claimed in claim 1 is characterized in that, the said metal chloride of step b is SnCl
22H
2O, CuCl
22H
2O, ZnCl
2, InCl
34H
2At least a among the O etc., solvent are at least a in deionized water, ethanol, terepthaloyl moietie, the hydrochloric acid.
4. the preparation method of a kind of preferred orientation ammonium chloride film as claimed in claim 1; It is characterized in that the substrate of the said even coating of step c is through the sol evenning machine spin coating; Sol evenning machine is with 200～3500 rev/mins of rotations; After then substrate being dried, so repeat once more 5～15 times, obtained certain thickness precursor thin-film sample.
5. the preparation method of a kind of preferred orientation ammonium chloride film as claimed in claim 1 is characterized in that, puts into 20～30 parts of hydrazine hydrates in the said encloses container of steps d.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012100625865A CN102602961A (en) | 2012-03-12 | 2012-03-12 | Method for preparing preferentially oriented ammonium chloride thin film |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012100625865A CN102602961A (en) | 2012-03-12 | 2012-03-12 | Method for preparing preferentially oriented ammonium chloride thin film |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103449841A (en) * | 2013-09-19 | 2013-12-18 | 山东建筑大学 | Preferred orientation ammonium chloride film |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3014815A (en) * | 1957-11-04 | 1961-12-26 | Philips Corp | Method of providing articles with metal oxide layers |
| CN101630701A (en) * | 2008-12-03 | 2010-01-20 | 山东建筑大学 | Method for preparing copper-indium-selenium optoelectronic thin film material of solar cell |
| CN102153288A (en) * | 2010-12-02 | 2011-08-17 | 山东建筑大学 | Method for preparing copper disulfide thin film with preferred orientation |
-
2012
- 2012-03-12 CN CN2012100625865A patent/CN102602961A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3014815A (en) * | 1957-11-04 | 1961-12-26 | Philips Corp | Method of providing articles with metal oxide layers |
| CN101630701A (en) * | 2008-12-03 | 2010-01-20 | 山东建筑大学 | Method for preparing copper-indium-selenium optoelectronic thin film material of solar cell |
| CN102153288A (en) * | 2010-12-02 | 2011-08-17 | 山东建筑大学 | Method for preparing copper disulfide thin film with preferred orientation |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103449841A (en) * | 2013-09-19 | 2013-12-18 | 山东建筑大学 | Preferred orientation ammonium chloride film |
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Application publication date: 20120725 |