CN103219420B - A kind of method of use four mischmetal preparation of target materials copper-zinc-tin-sulfur film - Google Patents

A kind of method of use four mischmetal preparation of target materials copper-zinc-tin-sulfur film Download PDF

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CN103219420B
CN103219420B CN201310100433.XA CN201310100433A CN103219420B CN 103219420 B CN103219420 B CN 103219420B CN 201310100433 A CN201310100433 A CN 201310100433A CN 103219420 B CN103219420 B CN 103219420B
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sputtering
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徐从康
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Ganzhou Youmo Technology Co., Ltd
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WUXI XUMATIC NEW ENERGY TECHNOLOGY Inc
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Abstract

The invention discloses a kind of method that use four mischmetal circular target prepares copper-zinc-tin-sulfur film, the method four mischmetal targets used are Cu 2znSnS 4, the method comprises the steps: (1) is heated to 300 ~ 400 DEG C by the glass-based base plate depositing molybdenum layer, adopts sputtering method, regulates sputtering power to 30 ~ 200W, and sputtering obtains ground floor film, and described ground floor film surface is the rich zinc state of poor copper; (2) regulate temperature to 400 ~ 600 DEG C of glass-based base plate, adopt sputtering method, regulate sputtering power to 80 ~ 200W, sputtering obtains second layer film, and described second layer film surface is rich copper state; (3) temperature regulating glass-based base plate is 400 ~ 600 DEG C, adopts sputtering method, regulates sputtering power to 30 ~ 200W, and sputtering obtains third layer film, and described third layer film surface is poor copper state, obtains copper-zinc-tin-sulfur film.

Description

A kind of method of use four mischmetal preparation of target materials copper-zinc-tin-sulfur film
Technical field
The present invention relates to a kind of preparation method of copper-zinc-tin-sulfur film, specifically relate to the method that employing four mischmetal circular target prepares copper-zinc-tin-sulfur film.
Background technology
Be classified as the most promising thin film solar cell technologies as by USDOE and other well-known solar cell research institutions, copper indium gallium selenium solar cell technology just by feat of its widely advantage attract increasing researcher and investor.Up to now, the efficiency of copper indium gallium selenium solar cell breaches 20.3% in the lab, suitable with monocrystalline silicon.Meanwhile, increasing company, mechanism are being devoted to trial production and the business extension of this technology.Such as, but the process of industrialization of copper indium gallium selenium solar cell still lags behind monocrystaline silicon solar cell and other thin-film solar cells, cadmium telluride thin-film battery at present.The biggest obstacle that current copper indium gallium selenium solar cell realizes scale of mass production is still its high production cost, therefore whole industry exigence searches out a kind of effective ways to overcome this obstacle, the scale of mass production cost of copper indium gallium selenium solar cell plate to be dropped to less than 1 dollar/watt, only have with abundant zinc, tin alternative rare element indium, the gallium respectively of mineral resources, thus can realize significantly reducing 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 just the same, copper-zinc-tin-sulfur (selenium) solar battery structure is also identical with copper indium gallium selenide cell structure.
The preparation method of copper-zinc-tin-sulfur (selenium) film is divided into vacuum and antivacuum method.At present most successful methods is antivacuum solwution method, and its efficiency can reach 11.1%, but owing to using poisonous diamine, can cause very large injury to environment.Evaporation coating method is the production method of the most effective copper indium gallium selenium solar cell altogether, 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 result is also not so good as hoped.Compared 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 because the vapour pressure of zinc-tin is high, be difficult to by four sources of routine or three source coevaporation methods the bulky grain crystalline form interface and high-quality copper-zinc-tin-sulfur (selenium) film that obtain the rich zinc of poor copper.
Summary of the invention
Technical problem to be solved by this invention is to provide the method for a kind of employing four mischmetal preparation of target materials copper-zinc-tin-sulfur films, and the 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:
Use four mischmetal circular target prepares a method for copper-zinc-tin-sulfur film, and the method four mischmetal circular target used are Cu 2znSnS 4, the method comprises the steps:
(1) the glass-based base plate depositing molybdenum layer is heated to 300 ~ 400 DEG C, regulates sputtering power to 30 ~ 200W, with circular target Cu 2znSnS 4sputter in substrate as sputtering target material and obtain ground floor film, 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 DEG C 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 ground floor thin film sputtering, sputtering time is 30min ~ 2h, and described second layer film surface is rich copper state;
(3) temperature regulating glass-based base plate is 400 ~ 600 DEG C, regulates sputtering power to 30 ~ 200W, with circular target Cu 2znSnS 4obtain third layer film as sputtering target material at second layer thin film sputtering, sputtering time is 20 ~ 60min, and described third layer film surface is poor copper state, obtains 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 4shape be disc.
Wherein, described four mischmetal circular target Cu 2znSnS 4diameter be 25,50,75,100 or 125 millimeters, thickness is 6 millimeters or 3 millimeters, described four mischmetal circular target Cu 2znSnS 4binding at thickness is on the copper base that 2-4 millimeter is identical with target diameter.
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, employs 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 four mischmetal sputtering target materials that the present invention adopts instead of traditional copper sulfide/copper/zinc and tin target, the formation of film can be controlled more accurately, thus guarantee uniformity of film, adopt four mischmetal sputtering target materials can also save or significantly shorten last vulcanisation step in addition, this is because the sulfur content in target is enriched, in whole step, the film obtained is in the atmosphere of sulfuration from the beginning to the end, therefore the after cure process needed for conventional sputter is not needed, thus greatly save heat energy, shorten the production time, reduce into product cost, protect environment.In addition, the most important innovative point of the present invention is unique copper zinc tin sulfur absorption layer structure: gradient-structure, absorbed layer connecting structure in the p-n on large-sized granular boundary and nanometer farmland, the present invention makes electronics and hole recombination rate reduce and then the efficiency of solar cell is got a promotion.
Accompanying drawing explanation
Fig. 1 is copper-zinc-tin-sulfur solar battery structure schematic diagram;
6. glass-based base plate; 5. molybdenum layer; 4.p-type copper zinc tin sulfur absorption layer; 3. cadmium sulfide or zinc sulphide resilient coating; 2. native oxide zinc; 1. transparent conductive oxide Window layer;
Fig. 2 is the flow chart that the present invention prepares copper-zinc-tin-sulfur film.
Embodiment
According to following embodiment, the present invention may be better understood.But those skilled in the art will readily understand, the content described by embodiment only for illustration of the present invention, and should can not limit the present invention described in detail in claims yet.
First copper-zinc-tin-sulfur film of the present invention need adopt evaporation or sputtering method to plate the metal molybdenum that a layer thickness is 200 ~ 1500 nanometers on base plate before being deposited on the glass-based base plate of 2 ~ 4 millimeters, the resistivity of molybdenum layer is 0.2 ~ 5 ohm.On copper-zinc-tin-sulfur (selenium) absorbed layer, the excessive layer of cadmium sulfide that a layer thickness is 40 ~ 250 nanometers is plated, temperature 150 ~ 250 degree of annealing 1 ~ 5 minute with chemical basin sedimentation (CBD) or atom deposition method (ALD).Then, plate native oxide zinc and aluminum zinc oxide transparency electrode with sputtering method or atomic layer deposition method, afterwards, evaporation plated electrode.In circular target technique, whole process be same circular target, by change electric current realize three-step approach.
Embodiment 1
The present invention's four mischmetal circular sputtering target materials used are Cu 2znSnS 4, target diameter is 75 millimeters, and thickness is, 6 millimeters, and atomicity is than being 2:1.5:0.5:4, and target bonding is 2.5 mm dias at thickness is on the copper base of 75 millimeters, and the method comprises the steps:
(1) adopt sputtering method, at thickness be 4mm glass-based base plate on plate molybdenum layer, sputtering condition is initial depression is 10 -6torr, the argon gas passing into 20SCCM make 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 depositing molybdenum layer is heated to 300 DEG C, regulates sputtering power to 30W, with circular target Cu 2znSnS 4sputter in substrate as sputtering target material and obtain ground floor film, sputtering time is 15min, and described ground floor film surface is the rich zinc state of poor copper;
(3) regulate the temperature to 400 DEG C of glass-based base plate, regulate sputtering power to 80W, with circular target Cu 2znSnS 4obtain second layer film as sputtering target material at ground floor thin film sputtering, sputtering time is 30min, and described second layer film surface is rich copper state;
(4) temperature regulating glass-based base plate is 400 DEG C, regulates sputtering power to 30W, with circular target Cu 2znSnS 4obtain third layer film as sputtering target material at second layer thin film sputtering, sputtering time is 20min, and described third layer film surface is poor copper state, obtains copper-zinc-tin-sulfur film.
(5) chemical basin sedimentation is adopted to plate cadmium sulfide transition zone on third layer film, obtain copper-zinc-tin-sulfur (selenium) film of overall poor copper, the thickness of described cadmium sulfide transition zone is 40nm, concrete operations are: after being mixed with the 28-30% ammoniacal liquor of 37.5ml by the distilled water of 240ml, add the sulphur urine mixing of the cadmium sulfate of 0.015mol33ml, 1.5mol16.5ml more successively, add the material that step (4) obtains, keep water temperature at 55-80 DEG C, and constantly stir 5min to 1h, then with distilled water cleaning several, dry up with nitrogen; Then anneal 1min under 150 DEG C of conditions.
Embodiment 2
The present invention's four mischmetal circular sputtering target materials used are Cu 2znSnS 4, target diameter is 25 millimeters, and thickness is 6 millimeters, and atomicity is than being 2:0.5:1.5:4, and target bonding is 3 mm dias at thickness is on the copper base of 25 millimeters, and the method comprises the steps:
(1) adopt sputtering method, at thickness be 2mm glass-based base plate on plate molybdenum layer, sputtering condition is initial depression is 10 -6torr, the argon gas passing into 20SCCM make 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 depositing molybdenum layer is heated to 350 DEG C, regulates sputtering power to 50W, with circular target Cu 2znSnS 4sputter in substrate as sputtering target material and obtain ground floor film, sputtering time is 30min, and described ground floor film surface is the rich zinc state of poor copper;
(3) regulate the temperature to 500 DEG C of glass-based base plate, regulate sputtering power to 120W, with circular target Cu 2znSnS 4obtain second layer film as sputtering target material at ground floor thin film sputtering, sputtering time is 60min, and described second layer film surface is rich copper state;
(4) temperature regulating glass-based base plate is 600 DEG C, regulates sputtering power to 50W, with circular target Cu 2znSnS 4obtain third layer film as sputtering target material at second layer thin film sputtering, sputtering time is 30min, and described third layer film surface is poor copper state, obtains copper-zinc-tin-sulfur film.
(5) chemical basin sedimentation is adopted to plate cadmium sulfide transition zone on third layer film, obtain copper-zinc-tin-sulfur (selenium) film of overall poor copper, the thickness of described cadmium sulfide transition zone is 150nm, concrete operations are: after being mixed with the 28-30% ammoniacal liquor of 37.5ml by the distilled water of 240ml, add the sulphur urine mixing of the cadmium sulfate of 0.015mol33ml, 1.5mol16.5ml more successively, add the material that step (4) obtains, keep water temperature at 55-80 DEG C, and constantly stir 5min to 1h, then with distilled water cleaning several, dry up with nitrogen; Then anneal 5min under 150 DEG C of conditions.
Embodiment 3
The present invention's four mischmetal circular sputtering target materials used are Cu 2znSnS 4, target diameter is, 100 millimeters, and thickness is 3 millimeters, and atomicity is than being 2:1.5:1.5:4, and target bonding is 4 mm dias at thickness is on the copper base of 100 millimeters, and the method comprises the steps:
(1) adopt method of evaporating, at thickness be 6mm glass-based base plate on plate molybdenum layer, evaporation conditions is initial vacuum degree 10 -6torr, voltage 7KV, electric current 20mA, evaporation time 30min, the thickness of described molybdenum layer is 1000nm, and the resistivity of described molybdenum layer is 1 ohmcm;
(2) the glass-based base plate depositing molybdenum layer is heated to 400 DEG C, regulates sputtering power to 70W, with circular target Cu 2znSnS 4sputter in substrate as sputtering target material and obtain ground floor film, sputtering time is 60min, and described ground floor film surface is the rich zinc state of poor copper;
(3) regulate the temperature to 550 DEG C of glass-based base plate, regulate sputtering power to 180W, with circular target Cu 2znSnS 4obtain second layer film as sputtering target material at ground floor thin film sputtering, sputtering time is 100min, and described second layer film surface is rich copper state;
(4) temperature regulating glass-based base plate is 500 DEG C, regulates sputtering power to 70W, with circular target Cu 2znSnS 4obtain third layer film as sputtering target material at second layer thin film sputtering, sputtering time is 60min, and described third layer film surface is poor copper state, obtains copper-zinc-tin-sulfur film.
(5) chemical basin sedimentation is adopted to plate cadmium sulfide transition zone on third layer film, obtain copper-zinc-tin-sulfur (selenium) film of overall poor copper, the thickness of described cadmium sulfide transition zone is 150nm, concrete operations are: after being mixed with the 28-30% ammoniacal liquor of 37.5ml by the distilled water of 240ml, add the sulphur urine mixing of the cadmium sulfate of 0.015mol33ml, 1.5mol16.5ml more successively, add the material that step (4) obtains, keep water temperature at 55-80 DEG C, and constantly stir 5min to 1h, then with distilled water cleaning several, dry up with nitrogen; Then anneal 5min under 150 DEG C of conditions.
Embodiment 4
The present invention's four mischmetal circular sputtering target materials used are Cu 2znSnS 4, target diameter is 125 millimeters, and thickness is 3 millimeters, and atomicity is than being 2:0.5:0.5:4, and target bonding is 2 mm dias at thickness is on the copper base of 125 millimeters, and the method comprises the steps:
(1) adopt method of evaporating, at thickness be 6mm glass-based base plate on plate molybdenum layer, evaporation conditions is initial vacuum degree 10 -6torr, voltage 7KV, electric current 20mA, evaporation time 30min, the thickness of described molybdenum layer is 1500nm, and the resistivity of described molybdenum layer is 0.2 ohmcm;
(2) the glass-based base plate depositing molybdenum layer is heated to 400 DEG C, regulates sputtering power to 200W, with circular target Cu 2znSnS 4sputter in substrate as sputtering target material and obtain ground floor film, sputtering time is 45min, and described ground floor film surface is the rich zinc state of poor copper;
(3) regulate the temperature to 600 DEG C of glass-based base plate, regulate sputtering power to 200W, with circular target Cu 2znSnS 4obtain second layer film as sputtering target material at ground floor thin film sputtering, sputtering time is 120min, and described second layer film surface is rich copper state;
(4) temperature regulating glass-based base plate is 450 DEG C, regulates sputtering power to 200W, with circular target Cu 2znSnS 4obtain third layer film as sputtering target material at second layer thin film sputtering, sputtering time is 45min, and described third layer film surface is poor copper state, obtains copper-zinc-tin-sulfur film.
(5) chemical basin sedimentation is adopted to plate cadmium sulfide transition zone on third layer film, obtain copper-zinc-tin-sulfur (selenium) film of overall poor copper, the thickness of described cadmium sulfide transition zone is 250nm, concrete operations are: after being mixed with the 28-30% ammoniacal liquor of 37.5ml by the distilled water of 240ml, add the sulphur urine mixing of the cadmium sulfate of 0.015mol33ml, 1.5mol16.5ml more successively, add the material that step (4) obtains, keep water temperature at 55-80 DEG C, and constantly stir 5min to 1h, then with distilled water cleaning several, dry up with nitrogen; Then anneal 3min under 250 DEG C of conditions.
Embodiment 5
By utilize embodiment 1 to 4 obtained copper-zinc-tin-sulfur film for the preparation of copper-zinc-tin-sulfur solar cell, and measure solar battery efficiency.The Current-voltage data of solar cell measures on Oriel solar simulator and Keithley2400 current source instrument, directly can obtain the efficiency of solar cell from self-editing LabviewI-V operating software, often organizes survey 3 times, the results are shown in Table 1.
The efficiency of the copper-zinc-tin-sulfur solar cell that table 1 utilizes the obtained copper-zinc-tin-sulfur film of embodiment 1 to 4 to obtain

Claims (6)

1. by a method for four mischmetal preparation of target materials copper-zinc-tin-sulfur films, it is characterized in that, the method four mischmetal circular target used are Cu 2znSnS 4, the method comprises the steps:
(1) the glass-based base plate depositing molybdenum layer is heated to 300 ~ 400 DEG C, regulates sputtering power to 30 ~ 200W, with circular target Cu 2znSnS 4sputter in substrate as sputtering target material and obtain ground floor film, 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 DEG C 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 ground floor thin film sputtering, sputtering time is 30min ~ 2h, and described second layer film surface is rich copper state;
(3) temperature regulating glass-based base plate is 400 ~ 600 DEG C, regulates sputtering power to 30 ~ 200W, with circular target Cu 2znSnS 4obtain third layer film as sputtering target material at second layer thin film sputtering, sputtering time is 20 ~ 60min, and described third layer film surface is poor copper state, obtains copper-zinc-tin-sulfur film.
2. use the method for four mischmetal preparation of target materials copper-zinc-tin-sulfur films according to claim 1, it is characterized in that, described target Cu 2znSnS 4atomicity than for 2:1:1:4.
3. use the method for four mischmetal preparation of target materials copper-zinc-tin-sulfur films according to claim 1, it is characterized in that, described target Cu 2znSnS 4shape be disc.
4. use the method for four mischmetal preparation of target materials copper-zinc-tin-sulfur films according to claim 1, it is characterized in that, described four mischmetal circular target Cu 2znSnS 4diameter be 25,50,75,100 or 125 millimeters, thickness is 6 millimeters or 3 millimeters, described four mischmetal target Cu 2znSnS 4binding at thickness is on the copper base that 2-4 millimeter is identical with target diameter.
5. use the method for four mischmetal preparation of target materials copper-zinc-tin-sulfur films according to claim 1, it is characterized in that, the thickness of described glass-based base plate is 2-6mm.
6. use the method for four mischmetal preparation of target materials copper-zinc-tin-sulfur films according to claim 1, it is characterized in that, the thickness of described molybdenum layer is 200 ~ 1500nm.
CN201310100433.XA 2013-03-26 2013-03-26 A kind of method of use four mischmetal preparation of target materials copper-zinc-tin-sulfur film Active CN103219420B (en)

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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
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
CN108155256B (en) * 2016-12-02 2020-03-10 北京有色金属研究总院 Copper-zinc-tin-sulfur thin-film solar cell with absorption layer having element gradient and preparation method thereof
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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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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