CN103219420A - Method for preparing Cu-Zn-Sn-S film from four-element alloy target material - Google Patents
Method for preparing Cu-Zn-Sn-S film from four-element alloy target material Download PDFInfo
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Abstract
The invention discloses a method for preparing a Cu-Zn-Sn-S film from a four-element alloy target material. The four-element alloy target material is Cu2ZnSnS4. The method comprises the following steps of (1), heating a glass base bottom plate with a molybdenum layer deposited to the temperature of 300 to 400 DEG C, using a sputtering method, adjusting the sputtering power to be 30 to 200W, and sputtering the glass base bottom plate to obtain a first layer of film, wherein the surface of the first layer of film is lack of copper and rich in zinc; (2), adjusting the temperature of the glass base bottom plate to be 400 to 600 DEG C, using the sputtering method, adjusting the sputtering power to be 80 to 200 W, and sputtering the glass base bottom plate to obtain a second layer of film, wherein the surface of the second layer of film is rich in copper; and (3), adjusting the temperature of the glass base bottom plate to be 400 to 600 DEG C, using the sputtering method, adjusting the sputtering power to be 30 to 200 W, and sputtering the glass base bottom plate to obtain a third layer of film, wherein the surface of the third layer of film is lack of copper, and then the Cu-Zn-Sn-S film is obtained.
Description
Technical field
The present invention relates to a kind of preparation method of copper-zinc-tin-sulfur film, specifically relate to adopt the circular target of quaternary element alloy to prepare the method for copper-zinc-tin-sulfur film.
Background technology
As being classified as the most promising thin film solar cell technologies by the well-known solar cell of USDOE and other research institution, the copper indium gallium selenium solar cell technology just by feat of its widely advantage attracting increasing researcher and investor.Up to now, the efficient of copper indium gallium selenium solar cell has broken through 20.3% in the laboratory, and is suitable with monocrystalline silicon.Simultaneously, increasing company, mechanism are being devoted to the trial production and the commercial extension of this technology.Yet the process of industrialization of copper indium gallium selenium solar cell still lags behind monocrystaline silicon solar cell and other thin-film solar cells, for example Cadimium telluride thin film battery at present.Copper indium gallium selenium solar cell realizes that the biggest obstacle of scale of mass production still is its high production cost at present, therefore whole industry exigence searches out a kind of effective ways and overcomes this obstacle, the scale of mass production cost of copper indium gallium selenium solar cell plate to be dropped to below 1 dollar/watt, have only with the abundant zinc of mineral resources, tin to substitute rare element indium, gallium respectively, thereby can realize reducing significantly the cost of raw material.The structure of matter of copper-zinc-tin-sulfur (selenium) and the structure of matter of Copper Indium Gallium Selenide are just the same, and copper-zinc-tin-sulfur (selenium) solar battery structure is also identical with the Copper Indium Gallium Selenide battery structure.
The preparation method of copper-zinc-tin-sulfur (selenium) film is divided into vacuum and antivacuum method.At present successful methods is antivacuum solwution method, and its efficient can reach 11.1%, but owing to use poisonous diamine, can cause very big injury to environment.Altogether evaporation coating method is the production method of effective copper indium gallium selenium solar cell, and it can obtain the copper indium gallium selenium solar cell of peak efficiency 20.3%.Because copper-zinc-tin-sulfur (selenium) has the structure same with Copper Indium Gallium Selenide, be expected to obtain high efficiency copper-zinc-tin-sulfur (selenium) solar cell with being total to vapour deposition method.But the result and not as hope.Compare with the achievement in research of the coevaporation of Copper Indium Gallium Selenide, the coevaporation achievement in research of copper-zinc-tin-sulfur (selenium) is few and few.This is the vapour pressure height because of zinc-tin, is difficult to obtain the bulky grain crystalline form interface and high-quality copper-zinc-tin-sulfur (selenium) film of the rich zinc of poor copper with four conventional sources or three source coevaporation methods.
Summary of the invention
Technical problem to be solved by this invention provides a kind of method that adopts quaternary element alloy target to prepare copper-zinc-tin-sulfur film, and this method can obtain the film of high-quality, high evenness.
For solving the problems of the technologies described above, the technical solution adopted in the present invention is:
A kind ofly prepare the method for copper-zinc-tin-sulfur film with the circular target of quaternary element alloy, the used circular target of quaternary element alloy of this method is Cu
2ZnSnS
4, this method comprises the steps:
(1) the glass-based base plate that will deposit molybdenum layer is heated to 300～400 ℃, regulates sputtering power to 30～200W, with circular target Cu
2ZnSnS
4Sputter in substrate obtains the ground floor film as sputtering target material, and sputtering time is 15～60min, and described ground floor film surface is the rich zinc state of poor copper;
(2) regulate temperature to 400～600 ℃ of glass-based base plate, regulate sputtering power to 80～200W, with circular target Cu
2ZnSnS
4Obtain second layer film as sputtering target material at the ground floor thin film sputtering, sputtering time is 30min～2h, and described second layer film surface is rich copper state;
(3) temperature of adjusting glass-based base plate is 400～600 ℃, regulates sputtering power to 30～200W, with circular target Cu
2ZnSnS
4Obtain three-layer thin-film as sputtering target material at second layer thin film sputtering, sputtering time is 20～60min, and described three-layer thin-film surface is poor copper state, promptly gets copper-zinc-tin-sulfur film.
Wherein, described target Cu
2ZnSnS
4Atomicity than for 1.5-2:(0.5-1.5): (0.5-1.5): 4.
Wherein, described target Cu
2ZnSnS
4Be shaped as disc.
Wherein, the circular target Cu of described quaternary element alloy
2ZnSnS
4Diameter be 25,50,75,100 or 125 millimeters, thickness is 6 millimeters or 3 millimeters, the circular target Cu of described quaternary element alloy
2ZnSnS
4Bonding is on the 2-4 millimeter copper base identical with the target diameter at thickness.
Wherein, the thickness of described glass-based base plate is 2-6mm.
Wherein, the thickness of described molybdenum layer is 200～1500nm.
Beneficial effect: what the present invention adopted is a kind of brand-new copper-zinc-tin-sulfur film manufacturing process, has used gradient-structure and interior absorbed layer connecting structure and single source sputtering technology, realizes the deposition of high efficiency battery core layer by changing base reservoir temperature and sputtering power.The quaternary element alloy sputtering target material that the present invention adopts has replaced traditional copper sulfide/copper/zinc and tin target; can control the formation of film more accurately; thereby assurance uniformity of film; adopt quaternary element alloy sputtering target material to save in addition or significantly shorten last vulcanisation step; this is because the sulfur content in the target is abundant; in whole steps; the film that obtains is in the atmosphere of sulfuration from the beginning to the end; therefore do not need the required after cure of conventional sputter to handle; thereby saved heat energy greatly; shorten the production time, reduced to become to produce cost, protected environment.In addition, the most important innovative point of the present invention is unique copper-zinc-tin-sulfur absorbent layer structure: gradient-structure, absorbed layer connecting structure in the p-n on large-sized granular boundary and nanometer farmland, the present invention reduces electronics and hole recombination rate and then the efficient of solar cell is got a promotion.
Description of drawings
Fig. 1 is a copper-zinc-tin-sulfur solar battery structure schematic diagram;
6. glass-based base plate; 5. molybdenum layer; 4.p-type copper-zinc-tin-sulfur absorbed layer; 3. cadmium sulfide or zinc sulphide resilient coating; 2. intrinsic zinc oxide; 1. transparent conductive oxide Window layer;
Fig. 2 prepares the flow chart of copper-zinc-tin-sulfur film for the present invention.
Embodiment
According to following embodiment, the present invention may be better understood.Yet, those skilled in the art will readily understand that the described content of embodiment only is used to illustrate the present invention, and should also can not limit the present invention described in detail in claims.
Copper-zinc-tin-sulfur film of the present invention at first needs to adopt on base plate evaporation or sputtering method to plate the metal molybdenum that a layer thickness is 200～1500 nanometers before being deposited on 2～4 millimeters glass-based base plate, and the resistivity of molybdenum layer is 0.2～5 ohm.On copper-zinc-tin-sulfur (selenium) absorbed layer, plate the excessive layer of cadmium sulfide that a layer thickness is 40～250 nanometers with chemical basin sedimentation (CBD) or atomic deposition method (ALD), temperature 150～250 degree annealing 1～5 minute.Then, plate intrinsic zinc oxide and aluminum zinc oxide transparency electrode with sputtering method or atomic layer deposition method, afterwards, the evaporation plated electrode.In circular target technology, what whole process was used is same circular target, realizes three-step approach by changing electric current.
The used circular sputtering target material of quaternary element alloy of the present invention is Cu
2ZnSnS
4, the target diameter is 75 millimeters, and thickness is, and 6 millimeters, atomicity is than being 2:1.5:0.5:4, and it is that 2.5 mm dias are that this method comprises the steps: on 75 millimeters the copper base that target binds at thickness
(1) adopting sputtering method, is to plate molybdenum layer on the glass-based base plate of 4mm at thickness, and sputtering condition is that initial depression is 10
-6The argon gas of Torr, feeding 20SCCM makes vacuum pressure reach 6mTorr, sputtering power 150W, sputtering time 45min, and the thickness of described molybdenum layer is 800nm, and the resistivity of described molybdenum layer is 3 ohmcms;
(2) the glass-based base plate that will deposit molybdenum layer is heated to 300 ℃, regulates sputtering power to 30W, with circular target Cu
2ZnSnS
4Sputter in substrate obtains the ground floor film as sputtering target material, and sputtering time is 15min, and described ground floor film surface is the rich zinc state of poor copper;
(3) regulate the temperature to 400 ℃ of glass-based base plate, regulate sputtering power to 80W, with circular target Cu
2ZnSnS
4Obtain second layer film as sputtering target material at the ground floor thin film sputtering, sputtering time is 30min, and described second layer film surface is rich copper state;
(4) temperature of adjusting glass-based base plate is 400 ℃, regulates sputtering power to 30W, with circular target Cu
2ZnSnS
4Obtain three-layer thin-film as sputtering target material at second layer thin film sputtering, sputtering time is 20min, and described three-layer thin-film surface is poor copper state, promptly gets copper-zinc-tin-sulfur film.
(5) adopt chemical basin sedimentation on three-layer thin-film, to plate the cadmium sulfide transition zone, promptly get copper-zinc-tin-sulfur (selenium) film of overall poor copper, the thickness of described cadmium sulfide transition zone is 40nm, concrete operations are: with the distilled water of 240ml with after the 28-30% ammoniacal liquor of 37.5ml mixes, add the cadmium sulfate of 0.015mol33ml, the sulphur urine mixing of 1.5mol16.5ml more successively, add the material that step (4) obtains, keep water temperature at 55-80 ℃, and constantly stir 5min to 1h, clean for several times with distilled water then, dry up with nitrogen; 1min then anneals under 150 ℃ of conditions.
The used circular sputtering target material of quaternary element alloy of the present invention is Cu
2ZnSnS
4, the target diameter is 25 millimeters, and thickness is 6 millimeters, and atomicity is than for 2:0.5:1.5:4, and it is that 3 mm dias are that this method comprises the steps: on 25 millimeters the copper base that target binds at thickness
(1) adopting sputtering method, is to plate molybdenum layer on the glass-based base plate of 2mm at thickness, and sputtering condition is that initial depression is 10
-6The argon gas of Torr, feeding 20SCCM makes vacuum pressure reach 6mTorr, sputtering power 150W, sputtering time 45min, and the thickness of described molybdenum layer is 200nm, and the resistivity of described molybdenum layer is 5 ohmcms;
(2) the glass-based base plate that will deposit molybdenum layer is heated to 350 ℃, regulates sputtering power to 50W, with circular target Cu
2ZnSnS
4Sputter in substrate obtains the ground floor film as sputtering target material, and sputtering time is 30min, and described ground floor film surface is the rich zinc state of poor copper;
(3) regulate the temperature to 500 ℃ of glass-based base plate, regulate sputtering power to 120W, with circular target Cu
2ZnSnS
4Obtain second layer film as sputtering target material at the ground floor thin film sputtering, sputtering time is 60min, and described second layer film surface is rich copper state;
(4) temperature of adjusting glass-based base plate is 600 ℃, regulates sputtering power to 50W, with circular target Cu
2ZnSnS
4Obtain three-layer thin-film as sputtering target material at second layer thin film sputtering, sputtering time is 30min, and described three-layer thin-film surface is poor copper state, promptly gets copper-zinc-tin-sulfur film.
(5) adopt chemical basin sedimentation on three-layer thin-film, to plate the cadmium sulfide transition zone, promptly get copper-zinc-tin-sulfur (selenium) film of overall poor copper, the thickness of described cadmium sulfide transition zone is 150nm, concrete operations are: with the distilled water of 240ml with after the 28-30% ammoniacal liquor of 37.5ml mixes, add the cadmium sulfate of 0.015mol33ml, the sulphur urine mixing of 1.5mol16.5ml more successively, add the material that step (4) obtains, keep water temperature at 55-80 ℃, and constantly stir 5min to 1h, clean for several times with distilled water then, dry up with nitrogen; 5min then anneals under 150 ℃ of conditions.
The used circular sputtering target material of quaternary element alloy of the present invention is Cu
2ZnSnS
4, the target diameter is, and 100 millimeters, thickness is 3 millimeters, and atomicity is than being 2:1.5:1.5:4, and it is that 4 mm dias are that this method comprises the steps: on 100 millimeters the copper base that target binds at thickness
(1) adopting method of evaporating, is to plate molybdenum layer on the glass-based base plate of 6mm at thickness, and evaporation conditions is initial vacuum degree 10
-6Torr, voltage 7KV, electric current 20mA, evaporation time 30min, the thickness of described molybdenum layer are 1000nm, the resistivity of described molybdenum layer is 1 ohmcm;
(2) the glass-based base plate that will deposit molybdenum layer is heated to 400 ℃, regulates sputtering power to 70W, with circular target Cu
2ZnSnS
4Sputter in substrate obtains the ground floor film as sputtering target material, and sputtering time is 60min, and described ground floor film surface is the rich zinc state of poor copper;
(3) regulate the temperature to 550 ℃ of glass-based base plate, regulate sputtering power to 180W, with circular target Cu
2ZnSnS
4Obtain second layer film as sputtering target material at the ground floor thin film sputtering, sputtering time is 100min, and described second layer film surface is rich copper state;
(4) temperature of adjusting glass-based base plate is 500 ℃, regulates sputtering power to 70W, with circular target Cu
2ZnSnS
4Obtain three-layer thin-film as sputtering target material at second layer thin film sputtering, sputtering time is 60min, and described three-layer thin-film surface is poor copper state, promptly gets copper-zinc-tin-sulfur film.
(5) adopt chemical basin sedimentation on three-layer thin-film, to plate the cadmium sulfide transition zone, promptly get copper-zinc-tin-sulfur (selenium) film of overall poor copper, the thickness of described cadmium sulfide transition zone is 150nm, concrete operations are: with the distilled water of 240ml with after the 28-30% ammoniacal liquor of 37.5ml mixes, add the cadmium sulfate of 0.015mol33ml, the sulphur urine mixing of 1.5mol16.5ml more successively, add the material that step (4) obtains, keep water temperature at 55-80 ℃, and constantly stir 5min to 1h, clean for several times with distilled water then, dry up with nitrogen; 5min then anneals under 150 ℃ of conditions.
The used circular sputtering target material of quaternary element alloy of the present invention is Cu
2ZnSnS
4, the target diameter is 125 millimeters, and thickness is 3 millimeters, and atomicity is than for 2:0.5:0.5:4, and it is that 2 mm dias are that this method comprises the steps: on 125 millimeters the copper base that target binds at thickness
(1) adopting method of evaporating, is to plate molybdenum layer on the glass-based base plate of 6mm at thickness, and evaporation conditions is initial vacuum degree 10
-6Torr, voltage 7KV, electric current 20mA, evaporation time 30min, the thickness of described molybdenum layer are 1500nm, the resistivity of described molybdenum layer is 0.2 ohmcm;
(2) the glass-based base plate that will deposit molybdenum layer is heated to 400 ℃, regulates sputtering power to 200W, with circular target Cu
2ZnSnS
4Sputter in substrate obtains the ground floor film as sputtering target material, and sputtering time is 45min, and described ground floor film surface is the rich zinc state of poor copper;
(3) regulate the temperature to 600 ℃ of glass-based base plate, regulate sputtering power to 200W, with circular target Cu
2ZnSnS
4Obtain second layer film as sputtering target material at the ground floor thin film sputtering, sputtering time is 120min, and described second layer film surface is rich copper state;
(4) temperature of adjusting glass-based base plate is 450 ℃, regulates sputtering power to 200W, with circular target Cu
2ZnSnS
4Obtain three-layer thin-film as sputtering target material at second layer thin film sputtering, sputtering time is 45min, and described three-layer thin-film surface is poor copper state, promptly gets copper-zinc-tin-sulfur film.
(5) adopt chemical basin sedimentation on three-layer thin-film, to plate the cadmium sulfide transition zone, promptly get copper-zinc-tin-sulfur (selenium) film of overall poor copper, the thickness of described cadmium sulfide transition zone is 250nm, concrete operations are: with the distilled water of 240ml with after the 28-30% ammoniacal liquor of 37.5ml mixes, add the cadmium sulfate of 0.015mol33ml, the sulphur urine mixing of 1.5mol16.5ml more successively, add the material that step (4) obtains, keep water temperature at 55-80 ℃, and constantly stir 5min to 1h, clean for several times with distilled water then, dry up with nitrogen; 3min then anneals under 250 ℃ of conditions.
The copper-zinc-tin-sulfur film that utilizes embodiment 1 to 4 to make is used to prepare the copper-zinc-tin-sulfur solar cell, and measures solar battery efficiency.The current-voltage data of solar cell are measured on Oriel solar simulator and Keithley2400 current source instrument, can directly obtain the efficient of solar cell from the self-editing Labview I-V operating software, survey 3 times, the results are shown in Table 1 for every group.
The efficient of the copper-zinc-tin-sulfur solar cell that the copper-zinc-tin-sulfur film that table 1 utilizes embodiment 1 to 4 to make obtains
Claims (6)
1. one kind prepares the method for copper-zinc-tin-sulfur film with the circular target of quaternary element alloy, it is characterized in that the used circular target of quaternary element alloy of this method is Cu
2ZnSnS
4, this method comprises the steps:
(1) the glass-based base plate that will deposit molybdenum layer is heated to 300～400 ℃, regulates sputtering power to 30～200W, with circular target Cu
2ZnSnS
4Sputter in substrate obtains the ground floor film as sputtering target material, and sputtering time is 15～60min, and described ground floor film surface is the rich zinc state of poor copper;
(2) regulate temperature to 400～600 ℃ of glass-based base plate, regulate sputtering power to 80～200W, with circular target Cu
2ZnSnS
4Obtain second layer film as sputtering target material at the ground floor thin film sputtering, sputtering time is 30min～2h, and described second layer film surface is rich copper state;
(3) temperature of adjusting glass-based base plate is 400～600 ℃, regulates sputtering power to 30～200W, with circular target Cu
2ZnSnS
4Obtain three-layer thin-film as sputtering target material at second layer thin film sputtering, sputtering time is 20～60min, and described three-layer thin-film surface is poor copper state, promptly gets copper-zinc-tin-sulfur film.
2. prepare the method for copper-zinc-tin-sulfur film according to claim 1 is described with the circular target of quaternary element alloy, it is characterized in that described target Cu
2ZnSnS
4Atomicity than for 2:(0.5-1.5): (0.5-1.5): 4.
3. prepare the method for copper-zinc-tin-sulfur film according to claim 1 is described with the circular target of quaternary element alloy, it is characterized in that described target Cu
2ZnSnS
4Be shaped as disc.
4. prepare the method for copper-zinc-tin-sulfur film according to claim 1 is described with the circular target of quaternary element alloy, it is characterized in that the circular target Cu of described quaternary element alloy
2ZnSnS
4Diameter be 25,50,75,100 or 125 millimeters, thickness is 6 millimeters or 3 millimeters, the circular target Cu of described quaternary element alloy
2ZnSnS
4Bonding is on the 2-4 millimeter copper base identical with the target diameter at thickness.
5. prepare the method for copper-zinc-tin-sulfur film according to claim 1 is described with the circular target of quaternary element alloy, it is characterized in that the thickness of described glass-based base plate is 2-6mm.
6. prepare the method for copper-zinc-tin-sulfur film according to claim 1 is described with the circular target of quaternary element alloy, it is characterized in that the thickness of described molybdenum layer is 200～1500nm.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103515482A (en) * | 2013-09-10 | 2014-01-15 | 华中科技大学 | Copper-indium-gallium-selenium thin film solar cell absorption layer and preparation method and application thereof |
| CN104282804A (en) * | 2014-09-03 | 2015-01-14 | 吉林化工学院 | Preparation method for adjusting element ratio of Cu2ZnSnS4 film through two times of sulfuration |
| CN104846342A (en) * | 2015-05-27 | 2015-08-19 | 清华大学 | Copper-zinc-tin-sulfur sputtering target and preparation method thereof |
| CN108155256A (en) * | 2016-12-02 | 2018-06-12 | 北京有色金属研究总院 | A kind of absorbed layer has copper-zinc-tin-sulfur film solar cell of graded elemental and preparation method thereof |
| CN109023275A (en) * | 2018-08-22 | 2018-12-18 | 昆明理工大学 | A kind of single target sputtering preparation Cu of binding3SnS4The method of absorbed layer |
Family Cites Families (3)
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| CN101452969B (en) * | 2008-12-29 | 2010-06-02 | 上海太阳能电池研究与发展中心 | Copper zincium tin sulfur compound semiconductor thin-film solar cell and manufacturing method |
| JP5745342B2 (en) * | 2011-06-03 | 2015-07-08 | ソーラーフロンティア株式会社 | CZTS thin film solar cell manufacturing method |
| CN102709393A (en) * | 2012-06-06 | 2012-10-03 | 成都先锋材料有限公司 | Method for preparing thin-film solar cells from copper-zinc-tin sulfur compound single target materials |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103515482A (en) * | 2013-09-10 | 2014-01-15 | 华中科技大学 | Copper-indium-gallium-selenium thin film solar cell absorption layer and preparation method and application thereof |
| CN104282804A (en) * | 2014-09-03 | 2015-01-14 | 吉林化工学院 | Preparation method for adjusting element ratio of Cu2ZnSnS4 film through two times of sulfuration |
| CN104282804B (en) * | 2014-09-03 | 2017-07-11 | 吉林化工学院 | It is a kind of that the preparation method that copper-zinc-tin-sulfur film element is matched is adjusted by post-cure |
| CN104846342A (en) * | 2015-05-27 | 2015-08-19 | 清华大学 | Copper-zinc-tin-sulfur sputtering target and preparation method thereof |
| CN108155256A (en) * | 2016-12-02 | 2018-06-12 | 北京有色金属研究总院 | A kind of absorbed layer has copper-zinc-tin-sulfur film solar cell of graded elemental and preparation method thereof |
| CN109023275A (en) * | 2018-08-22 | 2018-12-18 | 昆明理工大学 | A kind of single target sputtering preparation Cu of binding3SnS4The method of absorbed layer |
| CN109023275B (en) * | 2018-08-22 | 2020-07-31 | 昆明理工大学 | Preparation of Cu by binding single-target sputtering3SnS4Method of absorbing layer |
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