CN101820028A - Deposition method of multi-section camium sulfide thin film - Google Patents
Deposition method of multi-section camium sulfide thin film Download PDFInfo
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- CN101820028A CN101820028A CN201010111492A CN201010111492A CN101820028A CN 101820028 A CN101820028 A CN 101820028A CN 201010111492 A CN201010111492 A CN 201010111492A CN 201010111492 A CN201010111492 A CN 201010111492A CN 101820028 A CN101820028 A CN 101820028A
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Abstract
The invention relates to a deposition method of a multi-section camium sulfide thin film, comprising the following steps of: 1, placing a substrate containing a light-absorbing layer in first chemical bath solution with sulfide ions, cadmium ions and high bath temperature for depositing a first camium sulfide film on the light-absorbing layer of the substrate; and 2. placing the substrate into second chemical bath solution with sulfide ions, cadmium ions and low temperature for depositing a second camium sulfide film on the first camium sulfide film, wherein the temperature difference between the first chemical bath solution and the second chemical bath solution is above 10DEG C.
Description
Technical field
The present invention relates to a kind of cadmium sulfide thin film deposition method, particularly relate to a kind of deposition method of multi-section camium sulfide thin film.
Background technology
In recent years, the new line of and environmental consciousness surging with international oil price, green energy resource has become the new forms of energy main flow, wherein solar cell is again because of being the stable radiant energy of taking from the sun, the source can be inexhausted, and therefore more various countries pay attention to draw from one to make good the deficits of another invariably a large amount of development costs and subsidies granted for policy considerations, to foster local solar cell industry, make that the development of global solar industry is very quick.
First generation solar energy module comprises the solar energy module of monocrystalline silicon and polysilicon, though photoelectric conversion efficiency height and volume production technology maturation, because the material cost height, and Silicon Wafer influences follow-up volume production scale often because of the demand source of goods deficiency of semi-conductor industry.Therefore, comprise (CIGSS) thin-film solar module of the second generation of film and Cadimium telluride thin film of amorphous silicon membrane, Copper Indium Gallium Selenide (CIGS) film or Copper Indium Gallium Selenide (sulphur), in development and ripe gradually in recent years, wherein, therefore come into one's own especially again with the conversion efficiency of Copper Indium Gallium Selenide or Copper Indium Gallium Selenide (sulphur) solar cell the highest (element cell can up to 20% module about 14%).
Consult shown in Figure 1, the schematic diagram of existing located by prior art Copper Indium Gallium Selenide or Copper Indium Gallium Selenide (sulphur) solar battery structure.As shown in Figure 1, the copper indium gallium selenium solar cell structure of existing located by prior art comprises substrate 10, first conductive layer 20, Copper Indium Gallium Selenide or Copper Indium Gallium Selenide (sulphur) absorbed layer 30, resilient coating 40, the insulating barrier 50 and second conductive layer 60, wherein substrate 10 can be glass plate, aluminium sheet, Stainless Steel plate or plastic plate, first conductive layer 20 generally comprises metal molybdenum, be used as backplate, Copper Indium Gallium Selenide or Copper Indium Gallium Selenide (sulphur) absorbed layer 30 comprises the copper of proper proportion, indium, gallium and selenium, be used as p type film, be main light absorbed layer, resilient coating 40 can comprise cadmium sulfide (CdS), zinc sulphide (ZnS), zinc oxide (ZnO), zinc selenide (ZnSe), indium selenide (In
2Se
3) and indium sulfide (In
2S
3) etc., be used as n type film, insulating barrier 50 comprises zinc oxide (ZnO), in order to protection to be provided, second conductive layer 60 comprises zinc oxide aluminum (ZnO:Al), in order to connect front electrode.
In Copper Indium Gallium Selenide or Copper Indium Gallium Selenide (sulphur) solar battery structure, on Copper Indium Gallium Selenide or Copper Indium Gallium Selenide (sulphur) light absorbing zone, can plate the cadmium sulfide of the about 50～100nm of one deck, zinc sulphide, indium sulfide or indium selenide are as N layer or resilient coating, its film plating process comprises chemical bath deposition (chemical bathdeposition), microwave heating chemical bath deposition (microwave-assisted chemicalbath deposition), vacuum vapour deposition (vacuum evaporation), sputtering method (sputtering), chemical vapour deposition technique (chemical vapor deposition) and spray pyrolysis methods such as (spray pyrolysis), though there are many cushioning layer materials to use, but the Copper Indium Gallium Selenide or Copper Indium Gallium Selenide (sulphur) solar cell of coating cadmium sulfide resilient coating have optimum efficiency (about 20%), are still on the market material of the most normal use.
Existing known techniques can be plated the cadmium sulfide of the about 30～100nm of one deck thickness on Copper Indium Gallium Selenide or Copper Indium Gallium Selenide (sulphur) light absorbing zone, plating too thick meeting causes resistance too high, reduce solar battery efficiency, can cause light transmittance to descend simultaneously, influence light absorbing zone extinction amount, be easy to cover uneven and the big problem of each layer coverage rate difference and coating is too thin, so propose a kind of sedimentation of multi-stage cadmium sulfide, to improve above-mentioned shortcoming.
Summary of the invention
Main purpose of the present invention is, a kind of new deposition method of multi-section camium sulfide thin film is provided, technical problem to be solved is to make it utilize allotment different temperatures chemical bath, the substrate that will contain Copper Indium Gallium Selenide or Copper Indium Gallium Selenide (sulphur) light absorbing zone is inserted the immersion different time, makes to grow the different cadmium sulfide layer of characteristic.
The object of the invention to solve the technical problems realizes by the following technical solutions.A kind of deposition method of multi-section camium sulfide thin film according to the present invention's proposition, at least comprise following steps: step 1: place one to have sulphion and cadmium ion and the high first chemical bath solution of bathing temperature one substrate that contains light absorbing zone, with deposition one first cadmium sulphide film on the light absorbing zone of this substrate; And step 2: again aforesaid substrate is placed second a chemical bath solution with another low bath temperature of sulphion and cadmium ion, with deposition one second cadmium sulphide film on this first cadmium sulphide film, wherein the temperature contrast in this first chemical bath solution and the second chemical bath solution is more than 10 ℃.
The object of the invention to solve the technical problems also can be applied to the following technical measures to achieve further.
Aforesaid deposition method of multi-section camium sulfide thin film wherein in step 1, utilizes sulfur-containing compound and contains cadmium compound and purchase this chemical bath, and this chemical bath is adjusted into alkalescence.
Aforesaid deposition method of multi-section camium sulfide thin film wherein utilizes the ammoniacal liquor of concentration 20 to 30% to adjust the pH value of this chemical bath between 8 to 11.
Aforesaid deposition method of multi-section camium sulfide thin film, it further adds buffer and complexing agent in this chemical bath.
Aforesaid deposition method of multi-section camium sulfide thin film, wherein in step 1, this first chemical bath is bathed temperature between 75～90 ℃.
Aforesaid deposition method of multi-section camium sulfide thin film wherein in step 2, utilizes sulfur-containing compound and contains cadmium compound and purchase this another chemical bath, and this another chemical bath is adjusted into alkalescence, and this first chemical bath is bathed temperature between 60～75 ℃.
Aforesaid deposition method of multi-section camium sulfide thin film, the ammoniacal liquor that wherein utilizes concentration 20 to 30% with the pH value of another this chemical bath between 8 to 11.
Aforesaid deposition method of multi-section camium sulfide thin film, it further adds buffer and complexing agent in this another chemical bath.
Aforesaid deposition method of multi-section camium sulfide thin film, wherein said sulfur-containing compound are thiocarbamide (Thiourea), sulfuration acetamide (Thioacetamide) or sodium sulphate (Sodium sulfide); This contains cadmium compound is caddy (Cadmium Chloride), cadmium sulfate (Cadmium Sulfate), cadmium nitrate (Cadmium Nitrate), cadmium acetate (Cadmium Acetate) or cadmium iodide (CadmiumIodide).
The object of the invention to solve the technical problems also realizes by the following technical solutions.A kind of made multi-lamellar cadmium sulphide membrane of above-mentioned described deposition method of multi-section camium sulfide thin film of using according to the present invention's proposition.
The present invention compared with prior art has tangible advantage and beneficial effect.By technique scheme, deposition method of multi-section camium sulfide thin film of the present invention has following advantage and beneficial effect at least: multisection type coating of the present invention can improve the uneven problem that covers.
In sum, the present invention utilizes allotment different temperatures chemical bath, and the substrate that will contain Copper Indium Gallium Selenide or Copper Indium Gallium Selenide (sulphur) light absorbing zone is inserted the immersion different time, makes to grow the different cadmium sulfide layer of characteristic.The present invention has obvious improvement technically, has tangible good effect, really is a new and innovative, progressive, practical new design.
Above-mentioned explanation only is the general introduction of technical solution of the present invention, for can clearer understanding technological means of the present invention, and can be implemented according to the content of specification, and for above-mentioned and other purposes, feature and advantage of the present invention can be become apparent, below especially exemplified by preferred embodiment, and conjunction with figs., be described in detail as follows.
Description of drawings
Fig. 1 is the schematic diagram of prior art solar battery structure.
Fig. 2 is the process block diagram of deposition method of multi-section camium sulfide thin film of the present invention.
10: 20: the first conductive layers of substrate
30: absorbed layer 40: resilient coating
50: 60: the second conductive layers of insulating barrier
S101～S103: step
Embodiment
Reach technological means and the effect that predetermined goal of the invention is taked for further setting forth the present invention, below in conjunction with accompanying drawing and preferred embodiment, to its embodiment of deposition method of multi-section camium sulfide thin film, method, step, feature and the effect thereof that foundation the present invention proposes, describe in detail as after.
The present invention proposes a kind of deposition method of multi-section camium sulfide thin film, it provides a kind of chemical bath that utilizes different temperatures, to form the multilayer shape cadmium sulphide membrane that has different cadmium sulfide particles more than two-layer or two-layer, and can deposit the cadmium sulfide particle of different size because of the chemical bath of above-mentioned different temperatures, so deposition process of the present invention can be produced the preferable cadmium sulphide membrane of spreadability, so on using, can improve the efficient of solar cell.
Specific embodiments of the invention are earlier to be coated on the substrate by the slurry of the light absorbing zone of IB family, IIIA family and VIA family made, formation one contains the substrate of light absorbing zone, this absorbed layer can be Copper Indium Gallium Selenide (being called for short CIGS) or Copper Indium Gallium Selenide (sulphur) (being called for short CIGSS) absorbed layer, but do not exceed with above-mentioned, then aforesaid substrate is inserted in the chemical bath proposed by the invention, forming a kind of multilayer shape cadmium sulphide membrane at this solar energy absorbed layer, and then improve cadmium sulphide membrane and be covered in coverage effect on this light absorbing zone.
See also shown in Figure 2ly, at first, in step S101, place one to have sulphion and cadmium ion and the high first chemical bath solution of bathing temperature this substrate that contains light absorbing zone, with deposition one first cadmium sulphide film on the light absorbing zone of this substrate.In this step, mainly be to utilize sulphion, cadmium ion to form first cadmium sulphide film in proper additive and reaction condition deposit; In this specific embodiment, sulphion can be dissolved in the water and be provided by sulfur-containing compound, and sulfur-containing compound can be thiocarbamide (Thiourea), sulfuration acetamide (Thioacetamide) or sodium sulphate (Sodium sulfide), but does not exceed with above-mentioned; Cadmium ion then can be dissolved in the water and provides by containing cadmium compound, contain cadmium compound and can be caddy (Cadmium Chloride), cadmium sulfate (Cadmium Sulfate), cadmium nitrate (Cadmium Nitrate), cadmium acetate (Cadmium Acetate) or cadmium iodide (CadmiumIodide), but do not exceed with above-mentioned.Moreover, in the deposition step of phase I, form above-mentioned first cadmium sulphide film in order to make to deposit earlier on this light absorbing zone in large area, therefore, in this step, use high chemical bath of bathing temperature earlier, in this specific embodiment, the bath temperature of adjusting chemical bath is between 75～90 ℃, and the ammoniacal liquor that utilizes concentration 20 to 30% is adjusted into alkalescence with the pH value of this chemical bath, for example between 8 to 11, but not as limit.
On the other hand, in the deposition step of the phase I of step S101, more add buffer and complexing agent (complexing agent) in this chemical bath, for instance, buffer can be ammonium chloride, ammonium acetate, ammonium nitrate, ammonium sulfate etc.; And complexing agent can be ammoniacal liquor, three oneself join an aromatic plant metioned in ancient books ammonia (NTA), potassium cyanide (Potassium cyanide), triethanolamine (Triethanolamine, TEA), ethylenediamine (Ethylenediamine), ethylenediamine tetraacetic acid (EDTA) (EDTA), natrium citricum (sodium citrate) or the like.By this, this substrate that contains light absorbing zone is placed above-mentioned chemical bath, and cooperate stirring, after through the certain reaction sedimentation time (for example 1 to 20 minute), this first cadmium sulphide film can be deposited on the light absorbing zone of this substrate.
Then, step S103 further places aforesaid substrate one second chemical bath solution with another low bath temperature of sulphion and cadmium ion content again, with deposition one second cadmium sulphide film on this first cadmium sulphide film, because the chemical bath in this step has in the chemical bath than low temperature among the step S101, that is the bath temperature of first chemical bath is higher than the bath temperature of second chemical bath, and the actual temp difference is greater than more than 10 ℃, high entrained energy is higher because the temperature of bath temperature heals, sulphion and cadmium ion collision probability strengthens relatively, therefore its particle size of first cadmium sulphide film in the first warm chemical bath deposit of height bath is bigger, and its particle size of second cadmium sulphide film of the second chemical bath deposit of low bath temperature is less, so can fill up cadmium sulfide particle bigger in first cadmium sulphide film the zone that can't cover, gap between particles for example, therefore, the present invention can bathe the multi-lamellar cadmium sulphide membrane of temperature deposition varying particle size by difference, improves the spreadability of cadmium sulphide membrane for light absorbing zone.
The sulfur-containing compound that the step that coexists S101 is added, contain cadmium compound, the sulphion of the chemical bath in step S103 and cadmium ion can be respectively by thiocarbamide, sulfuration acetamide or sodium sulphate, and caddy, cadmium sulfate, cadmium nitrate, cadmium acetate or cadmium iodide be dissolved in the solvent and form, but do not exceed with above-mentioned.And the bath temperature of the chemical bath of the deposition step of this second stage is between 60～75 ℃.
Similarly, the chemical bath of step S103 also is added with buffer, complexing agent etc., and the ammoniacal liquor that also utilizes concentration 20 to 30% is adjusted into alkalescence with the pH value of the chemical bath of step S103, for example between 8 to 11, implements aspect in detail and can consult explanation among the step S101.Certainly, in step S103, also can carry out suitable adjustment at relevant parameter, for example substrate is placed the time of second chemical bath to be shortened or reduce the temperature of the chemical bath of step S103, and then deposit size conforms and insert position, the intergranular space of cadmium sulfide in first cadmium sulphide film.
By the substrate after the step S101 is inserted the chemical bath that step S103 is allocated, after one period reaction time, promptly can form second cadmium sulphide film on first cadmium sulphide film.And through after the concrete experiment of the present invention, the bath temperature difference of gentle second chemical bath of the bath of this first chemical bath is different best more than 10 ℃, make the cadmium sulfide particle of second cadmium sulphide film can fill up in the hole of first cadmium sulphide film, to improve the whole covering power of cadmium sulphide membrane.
It should be noted that, in the above-mentioned specific embodiment, be to utilize two stage different chemical bath deposition multilayer shape of the present invention cadmium sulphide membrane of bathing temperature, but the chemical deposition that more extensible two stages of explanation of aspect of the present invention are above, and the difference of bath temperature that makes the different depositional phases is more than 10 ℃, have the difference in size opposite sex with the cadmium sulfide particle of reaching interlayer, and then improve the spreadability of cadmium sulphide membrane.For example ground floor be 85～95 ℃ of deposit, the second layer in middle temperature at high temperature is that 75～85 ℃ of deposit, the 3rd layer are 65～75 ℃ of deposit at low temperature, by that analogy, Chen Ji different layers film in this way, can reach the particle size otherness of different layers, reach the purpose that improves spreadability.
Simultaneously the total content of cadmium ion is 10～500 times of cadmium content in the cadmium sulphide membrane in the chemical bath, and the total content of sulphion is 5～100 times of sulfur content in the cadmium sulphide membrane.The concentration of ammoniacal liquor is 20～30%, and the optimal pH of chemical bath is pH8～11.
The above, it only is preferred embodiment of the present invention, be not that the present invention is done any pro forma restriction, though the present invention discloses as above with preferred embodiment, yet be not in order to limit the present invention, any those skilled in the art, in not breaking away from the technical solution of the present invention scope, when the technology contents that can utilize above-mentioned announcement is made a little change or is modified to the equivalent embodiment of equivalent variations, in every case be not break away from the technical solution of the present invention content, according to technical spirit of the present invention to any simple modification that above embodiment did, equivalent variations and modification all still belong in the scope of technical solution of the present invention.
Claims (10)
1. deposition method of multi-section camium sulfide thin film, its feature is in comprising following steps at least:
Step 1: place one to have sulphion and cadmium ion and the high first chemical bath solution of bathing temperature one substrate that contains light absorbing zone, with deposition one first cadmium sulphide film on the light absorbing zone of this substrate; And
Step 2: again aforesaid substrate is placed second a chemical bath solution with another low bath temperature of sulphion and cadmium ion, with deposition one second cadmium sulphide film on this first cadmium sulphide film, wherein the temperature contrast in this first chemical bath solution and the second chemical bath solution is more than 10 ℃.
2. deposition method of multi-section camium sulfide thin film according to claim 1 is characterized in that wherein utilizing sulfur-containing compound and containing cadmium compound and to purchase this chemical bath, and this chemical bath is adjusted into alkalescence in step 1.
3. deposition method of multi-section camium sulfide thin film according to claim 2 is characterized in that wherein utilizing the ammoniacal liquor of concentration 20 to 30% to adjust the pH value of this chemical bath between 8 to 11.
4. deposition method of multi-section camium sulfide thin film according to claim 3 is characterized in that it further adds buffer and complexing agent in this chemical bath.
5. deposition method of multi-section camium sulfide thin film according to claim 4 is characterized in that wherein in step 1, and this first chemical bath is bathed temperature between 75～90 ℃.
6. deposition method of multi-section camium sulfide thin film according to claim 5, it is characterized in that wherein in step 2, utilize sulfur-containing compound and contain cadmium compound and purchase this another chemical bath, and this another chemical bath is adjusted into alkalescence, and this first chemical bath is bathed temperature between 60～75 ℃.
7. deposition method of multi-section camium sulfide thin film according to claim 6, the ammoniacal liquor that it is characterized in that wherein utilizing concentration 20 to 30% with the pH value of another this chemical bath between 8 to 11.
8. deposition method of multi-section camium sulfide thin film according to claim 7 is characterized in that it further adds buffer and complexing agent in this another chemical bath.
9. according to claim 2 or 6 described deposition method of multi-section camium sulfide thin film, it is characterized in that wherein said sulfur-containing compound is thiocarbamide, sulfuration acetamide or sodium sulphate; This contains cadmium compound is caddy, cadmium sulfate, cadmium nitrate, cadmium acetate or cadmium iodide.
10. use the made multi-lamellar cadmium sulphide membrane of deposition method of multi-section camium sulfide thin film as claimed in claim 1 for one kind.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102299211A (en) * | 2011-09-21 | 2011-12-28 | 上海大学 | Two-step method for manufacturing cadmium sulphide film |
| CN103443929A (en) * | 2010-12-27 | 2013-12-11 | 凸版印刷株式会社 | Compound semiconductor thin film solar cell, and process for production thereof |
| CN106159038A (en) * | 2015-05-15 | 2016-11-23 | 北京铂阳顶荣光伏科技有限公司 | Hexagonal phase extension cadmium sulfide in the copper indium gallium selenide of photovoltaic junction |
| CN110177900A (en) * | 2017-12-20 | 2019-08-27 | 北京铂阳顶荣光伏科技有限公司 | Mead-Bauer recovery system, chemical bath deposition device and its deposition method |
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| US20050236032A1 (en) * | 2002-03-26 | 2005-10-27 | Satoshi Aoki | Compound thin-film solar cell and process for producing the same |
| US20090255461A1 (en) * | 2006-04-13 | 2009-10-15 | Solopower, Inc. | Apparatus for Simultaneous Roll-to-Roll Wet Processing of Two Workpieces Disposed Within a Single Chamber |
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| US20050236032A1 (en) * | 2002-03-26 | 2005-10-27 | Satoshi Aoki | Compound thin-film solar cell and process for producing the same |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103443929A (en) * | 2010-12-27 | 2013-12-11 | 凸版印刷株式会社 | Compound semiconductor thin film solar cell, and process for production thereof |
| CN102299211A (en) * | 2011-09-21 | 2011-12-28 | 上海大学 | Two-step method for manufacturing cadmium sulphide film |
| CN106159038A (en) * | 2015-05-15 | 2016-11-23 | 北京铂阳顶荣光伏科技有限公司 | Hexagonal phase extension cadmium sulfide in the copper indium gallium selenide of photovoltaic junction |
| US10446706B2 (en) | 2015-05-15 | 2019-10-15 | Beijing Apollo Ding Rong Solar Technology Co., Ltd. | Hexagonal phase epitaxial cadmium sulfide on copper indium gallium selenide for a photovoltaic junction |
| CN106159038B (en) * | 2015-05-15 | 2020-02-11 | 北京铂阳顶荣光伏科技有限公司 | Hexagonal phase epitaxial cadmium sulfide on copper indium gallium selenide for photovoltaic junction |
| CN110177900A (en) * | 2017-12-20 | 2019-08-27 | 北京铂阳顶荣光伏科技有限公司 | Mead-Bauer recovery system, chemical bath deposition device and its deposition method |
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Application publication date: 20100901 |