CN101645473B - Preparation method of selenide material for absorbing layer of thin film solar cell - Google Patents
Preparation method of selenide material for absorbing layer of thin film solar cell Download PDFInfo
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- CN101645473B CN101645473B CN2009103067939A CN200910306793A CN101645473B CN 101645473 B CN101645473 B CN 101645473B CN 2009103067939 A CN2009103067939 A CN 2009103067939A CN 200910306793 A CN200910306793 A CN 200910306793A CN 101645473 B CN101645473 B CN 101645473B
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Abstract
The invention relates to a preparation method of selenide material for the absorbing layer of a thin film solar cell and the selenide material is Cu2Sex and M2Sey, wherein M is one element of Al, In and Ga, x is 0.95-1.05, y is 2.8-3.2 and selenide material is powdered or block target material. The preparation method comprises the following steps: placing a sealed vacuum container or a container filled with argon or nitrogen with the pressure of less than normal pressure in a furnace to perform gradient temperature-elevating and temperature-keeping in a defined heating rate, performing liquidphase cooling to synthesize bulk material after stage temperature-keeping, crushing the bulk material to obtain the desired powder and finally synthesizing the desired bulk target in a hot pressing furnace. The method is a pure element method liquid-phase synthesis technology and has the advantage of wide applicability, accurate proportioning and low cost; the prepared target has high quality andthe consistencies of the powdery material and the bulk target material are separately more than 99.7% and 99.0%.
Description
Technical field
The present invention relates to a kind of preparation method of selenide material for absorbing layer of thin film solar cell, described selenide material is Cu
2Se
x, In
2Se
y, Al
2Se
y, Ga
2Se
y, the value of x is 0.95～1.05, and the value of y is 2.8～3.2, and the materials behavior of preparation is powder or block target.
Background technology
CuAlSe
2, CuInSe
2, Cu (InGa) Se
2, Cu (AlGa) Se
2As light absorbing zone, have the characteristics of radioresistance, stable performance, can be prepared into lower-cost solar film battery, be fit to civilian, the present mature methods of its preparation method generally adopts selenizing after the first sputter (or sulfuration) technology, this method can not guarantee the uniformity of thin film composition and thickness, and selenizing technology relates to hypertoxic selenides (or sulfide), and is higher to equipment requirements in preparation process.In order to simplify technology and to reduce cost, American scholar is utilized the CuInGaSe target, method by a step sputter has prepared CIGS light absorbing zone (C.Suryanarayanaa, E.Ivanovb, R.Nou, M.A.Contrerasc, J.J.Moore Synthesis and processing of a Cu-In-Ga-Se sputtering target, Thin Solid Films, 1998 v332. 340-344), this technology has been simplified preparation flow greatly, can accurately control thin film composition and thickness, makes selenizing work simplification even cancellation.
Such as draw a bow of people from Tsing-Hua University utilizes Cu
2Se, In
2Se
3, Al
2Se
3, Ga
2Se
3Powder synthesizes CuAlSe
2, CuInSe
2, Cu (InGa) Se
2, Cu (AlGa) Se
2(a kind of technology patent publication No. for preparing copper-indium-selenium sputtering target such as draw a bow target: CN 101333645A; Copper Indium Gallium Selenide such as Zhuan Daming or Cu-In-Al-Se solar cell absorption layer target material and preparation method thereof patent publication No.: CN 101397647A), the Korea S scholar utilizes Cu
2Se, In
2Se
3, Cu
2S, In
2S
3Target has synthesized the CuInGaSSe film.(Kyoo-Ho Kim, Effect of Ga, S Additions in CulnSe2 for Solar Cell Applications, J Kor. Inst. Sur. Eng. V58 (4), 2004, P191-195), use Cu
2Se, In
2Se
3, Al
2Se
3, Ga
2Se
3Target built up membrane solar battery obsorbing layer is a feasible method.
Therefore, Cu
2Se, In
2Se
3, Al
2Se
3, Ga
2Se
3Powder becomes the critical material of preparation respective films solar cell absorption layer target material.Fusing point, boiling point, the density contrast opposite sex between Cu, In, Ga, Al, five elements of Se is very big, and (its fusing point is respectively 1083.4 ℃, 156.6 ℃, 29.7 ℃, 660.4 ℃ and 217 ℃; Its boiling point is respectively 2567 ℃, 2080 ℃, 2204 ℃, 2467 ℃ and 684.9 ℃; Its density is respectively 8.96g/cm
3, 7.3g/cm
3, 5.9g/cm
3, 4.8g/cm
3, 2.7g/cm
3), especially: the boiling point of selenium not only low (684.9 ℃), and its vapour pressure when boiling point very high (1 * 10
5Pa), cause floating at alloy surface of a large amount of volatilizations of Se and Se in the alloy preparation process easily, make its can not be fully and alloy merge, be difficult to form integrated alloy; Also have selenium and Ga, In that violent chemical reaction takes place, preparation technology designs unreasonable, causes the breaking-up of equipment, the pollution of environment and the loss of selenium easily.Therefore, volatilization and the even distribution of Se in alloy of control Se are that difficult point also is crucial.
Summary of the invention
The technical problem to be solved in the present invention is: a kind of preparation method of selenide material for absorbing layer of thin film solar cell is provided, and this method is a kind of pure element method, with gradient increased temperature constant temperature, liquid phase cools synthesis technique, prepares fusing point, In that density is suitable
2Se
3, Ga
2Se
3, Al
2Se
3, (its fusing point is respectively 880 ℃, 1020 ℃, 950 ℃, 1120 ℃ to intermediate compound such as CuSe; Its density is respectively 5.67g/cm
3, 4.92 g/cm
3, 5.03 g/cm
3, 5.99 g/cm
3), volatilization and the selenium and the abundant alloying problem of other element of solution selenium, it is wide to have applicability, proportion speed, cost is low, the target quality height of preparation, the density of dusty material reaches more than 99.7%, and block target density reaches the advantage more than 99.0%.
The technical scheme that solves its above-mentioned technical problem is: a kind of selenide material for absorbing layer of thin film solar cell preparation method, described selenide material is Cu
2Se
x, M
2Se
y, wherein M for or be selected from a kind of element among Al, In, the Ga, the value of x is 0.95～1.05, the value of y is 2.8～3.2, the preparation of above-mentioned selenide material may further comprise the steps:
A. required element material is put into container after by material composition requirement proportioning, less than 10
-2Under the Pa vacuum degree condition closed container or under the condition that charges into the argon gas, nitrogen or the helium that are lower than atmospheric pressure closed container;
B. airtight container is placed and be gradient increased temperature constant temperature in the stove, promptly with the heating rate of 10～20 ℃/min, be divided into 4～5 sections intensification constant temperature according to adjusting to the temperature that is higher than material melting point at last, each temperature section temperature is: the temperature that is higher than material melting point/(4～5)+1 of (30～+ 30) ℃+adjust at last, constant temperature time was respectively 2～4 hours, end temperature is adjusted under the temperature that is higher than material melting point and is incubated 0.1 hour～10 hours, make its slow cool to room temperature in 8 hours, the block of preparation is taken out the back ball milling in container, with powder sieving, obtain powder-product;
C. the powder of preparing is put into hot pressing furnace mould on demand dimensioned after 500 ℃～900 ℃, 30MPa～300MPa compacting and promptly obtained required block target.
Further technical scheme of the present invention is: when needed product is powder, and cancellation step C.
Further technical scheme of the present invention is: the temperature that is higher than material melting point described in the step B is 900 ℃～1250 ℃.
The preparation method of a kind of selenide material for absorbing layer of thin film solar cell of the present invention, accurate in order to satisfy the solar cell industry exactly to composition proportion, high-purity solar battery obsorbing layer is to the demand of selenide material and the technology of developing, and it has following beneficial effect:
1, applicability is wide: the Cu that can prepare the heterogeneity proportioning
2Se
x, In
2Se
y, Al
2Se
y, Ga
2Se
y, the value of x is 0.95～1.05, the value of y is 2.8～3.2, the material property of preparing is stable, and the materials behavior of preparation is powder or block target, and the materials behavior of preparation is powder or block target, powder can be used for multicomponent target material, and the block target can be used for sputter coating.
2, proportion speed: the material of acquisition is difficult for introducing impurity, composition is even, element ratio is easy to control, proportion speed.
3, cost is low: this technology can prepare large-area target, and can make in batches.
4, target quality height: owing to adopt vacuum tightness synthetic, hot pressed sintering, the target even compact that obtains, the density of dusty material reaches more than 99.7%, and block target density reaches more than 99.0%, the film even film layer that obtains, smooth, strong adhesion.
Below, the technical characterictic to the preparation method of the present invention's selenide material for absorbing layer of thin film solar cell is further described in conjunction with the accompanying drawings and embodiments.
Description of drawings
Fig. 1: preparation method's flow chart of the present invention's selenide material for absorbing layer of thin film solar cell.
Embodiment
Embodiment 1
With Cu powder, the Se piece of purity 99.995%, behind Cu:Se=2:1 proportioning 400g, put into the autoclave of liner aluminium oxide ceramics, in molar ratio 7 * 10
-3Seal autoclave under the Pa vacuum degree condition.
Autoclave placed and the nitrogen circulation cooling arranged, and the furnace wall also has in the stove of recirculated water cooling, in the stove is gradient increased temperature constant temperature, promptly with the heating rate of 10 ℃/min, be divided into 5 sections intensification constant temperature for 1200 ℃ according to adjusting to the temperature that is higher than material melting point at last, the temperature of each temperature section is: the temperature/5+1 that is higher than material melting point that adjusts at last, promptly 5 sections thermostat temperatures are respectively 200 ℃, 400 ℃, 600 ℃, 800 ℃, 1000 ℃, constant temperature time was respectively 2 hours, the temperature conditions that is adjusted to 1200 ℃ at last is incubated 2 hours down, makes its slow cool to room temperature in 8 hours.The block of preparation is taken out the back ball milling in autoclave, powder sieving is become-400 purpose grades, obtain Cu
2The Se powder, powder purity is greater than 99.99%.
The powder of preparing is put into diameter 80mm mould at the target that is processed into diameter 75mm under 800 ℃, 150MPa condition after with the hot-pressed sintering furnace compacting.The target density can reach 99.3%.
Embodiment 2
With Cu powder, the Se piece of purity 99.98%, behind Cu:Se=2:1.05 proportioning 1500g, put into the reactor of liner aluminium oxide ceramics in molar ratio, charge into 8 * 10
4Pa argon gas capping still.
It is gradient increased temperature constant temperature that the reactor that charges into argon gas is placed in the stove, promptly with the heating rate of 15 ℃/min, be divided into 5 sections intensification constant temperature for 1210 ℃ according to adjusting to the temperature that is higher than material melting point at last, the temperature of each temperature section is :-12+ ℃ of temperature/the 5+1 that is higher than material melting point that adjusts at last, promptly 5 sections thermostat temperatures are respectively 190 ℃, 380 ℃, 570 ℃, 760 ℃, 950 ℃, constant temperature time: 2.5 hours, the temperature conditions that is adjusted to 1210 ℃ at last is incubated 2.5 hours down, makes its slow cool to room temperature in 8 hours.The block of preparation is taken out the back ball milling in reactor, powder sieving is become-300 purpose grades, obtain Cu
2Se
1.05Powder.Powder purity is greater than 99.95%.
The powder of preparing is put into diameter 350mm mould at the target that is processed into diameter 310mm under 850 ℃, 120MPa condition after with the hot-pressed sintering furnace compacting.The target density can reach 99.1%.
Embodiment 3
With In piece, the Se piece of purity 99.8%, behind In:Se=2:3 proportioning 500g, put into the autoclave of liner zirconia ceramics, in molar ratio 6.2 * 10
-3Seal autoclave under the Pa vacuum degree condition.
The autoclave that seals under the vacuum placed and the nitrogen circulation cooling arranged, and the furnace wall also has in the stove of recirculated water cooling, in the stove is gradient increased temperature constant temperature, promptly with the heating rate of 20 ℃/min, be divided into 4 sections intensification constant temperature for 950 ℃ according to adjusting to the temperature that is higher than material melting point at last, the temperature of each temperature section is: 10 ℃+temperature/4+1 that is higher than material melting point that adjusts at last, promptly 4 sections thermostat temperatures are respectively 200 ℃, 400 ℃, 600 ℃, 800 ℃, constant temperature time was respectively 3 hours, the temperature conditions that is adjusted to 950 ℃ at last is incubated 4 hours down, makes its slow cool to room temperature in 8 hours.The block of preparation is taken out the back ball milling in autoclave, powder sieving is become-200 purpose grades, obtain In
2Se
3Powder.Powder purity is greater than 99.7%.
The powder of preparing is put into diameter 110mm mould at the target that is processed into diameter 100mm under 600 ℃, 160MPa condition after with the hot-pressed sintering furnace compacting.The target density can reach 99.3%.
Embodiment 4
With In piece, the Se piece of purity 99.998%, behind the In:Se=2:3.1 proportioning 800g, put into the retort of enamel in molar ratio, charge into 9 * 10
3Pa nitrogen closing reactor.
It is gradient increased temperature constant temperature that the reactor that charges into nitrogen is placed in the stove, promptly with the heating rate of 20 ℃/min, be divided into 4 sections intensification constant temperature for 900 ℃ according to adjusting to the temperature that is higher than material melting point at last, the temperature of each temperature section is: the temperature/4+1 that is higher than material melting point of (5～5) ℃+adjust at last, promptly 4 sections thermostat temperatures are respectively 175～185 ℃, 350～370 ℃, 525～555 ℃, 700～740 ℃, constant temperature time was respectively 2 hours, the temperature conditions that is adjusted to 900 ℃ at last is incubated 3 hours down, makes its slow cool to room temperature in 8 hours.The block of preparation is taken out the back ball milling in reactor, powder sieving is become-400 purpose grades, obtain In
2Se
3.1Powder.Powder purity is greater than 99.997%.
The powder of preparing is put into diameter 150mm mould at the target that is processed into diameter 145mm under 630 ℃, 200MPa condition after with the hot-pressed sintering furnace compacting.The target density can reach 99.8%.
Embodiment 5
With Al powder, the Se piece of purity 99.91%, behind the Al:Se=2:3 proportioning 900g, put into the reactor of liner aluminium oxide ceramics, in molar ratio 4 * 10
-3Seal reactor under the Pa vacuum degree condition.
It is gradient increased temperature constant temperature that sealing under the vacuum is placed in the stove, promptly with the heating rate of 12 ℃/min, be divided into 5 sections intensification constant temperature for 1020 ℃ according to adjusting to the temperature that is higher than material melting point at last, the temperature of each temperature section is :-30 ℃+temperature/5+1 that is higher than material melting point that adjusts at last, promptly 5 sections thermostat temperatures are respectively 140 ℃, 280 ℃, 420 ℃, 560 ℃, 700 ℃, constant temperature time was respectively 2.5 hours, the temperature conditions that is adjusted to 1020 ℃ at last is incubated 3.5 hours down, makes its slow cool to room temperature in 8 hours.The block of preparation is taken out the back ball milling in reactor, powder sieving is become-300 purpose grades, obtain Al
2Se
3Powder, powder purity is greater than 99.9%.
The powder of preparing is put into diameter 160mm mould at the target that is processed into diameter 150mm under 650 ℃, 180MPa condition after with the hot-pressed sintering furnace compacting.The target density can reach 99.6%.
Embodiment 6
With Al powder, the Se piece of purity 99.995%, behind Al:Se=2:3.2 proportioning 400g, put into the pressure pan of liner aluminium oxide ceramics, in molar ratio 7 * 10
-3Seal autoclave under the Pa vacuum degree condition.
It is gradient increased temperature constant temperature that autoclave is placed in the stove, promptly with the heating rate of 18 ℃/min, be divided into 5 sections intensification constant temperature for 1010 ℃ according to adjusting to the temperature that is higher than material melting point at last, the temperature of each temperature section is :-10 ℃+temperature/5+1 that is higher than material melting point that adjusts at last, promptly 5 sections thermostat temperatures are respectively 158 ℃, 316 ℃, 474 ℃, 632 ℃, 790 ℃, constant temperature time was respectively 2 hours, the insulation 2 hours down of the temperature conditions of last adjustment to 1010 ℃ makes its slow cool to room temperature in 8 hours.The block of preparation is taken out the back ball milling in autoclave, powder sieving is become-400 purpose grades, obtain Al
2Se
3.2Powder.Powder purity is greater than 99.99%.
The powder of preparing is put into diameter 80mm mould at the target that is processed into diameter 75mm under 700 ℃, 150MPa condition after with the hot-pressed sintering furnace compacting.The target density can reach 99.3%.
Embodiment 7
With Ga piece, the Se piece of purity 99.98%, behind Ga:Se=2:3 proportioning 1500g, put into the reactor of liner aluminium oxide ceramics in molar ratio, charge into 7 * 10
4Pa argon gas capping still.
It is gradient increased temperature constant temperature that the reactor that charges into argon gas is placed in the stove, promptly with the heating rate of 10 ℃/min, be divided into 4 sections intensification constant temperature for 950 ℃ according to adjusting to the temperature that is higher than material melting point at last, the temperature of each temperature section is: 20 ℃+temperature/4+1 that is higher than material melting point that adjusts at last, promptly 4 sections thermostat temperatures are respectively 210 ℃, 420 ℃, 630 ℃, 840 ℃, constant temperature time was respectively 2.5 hours, the temperature conditions that is adjusted to 950 ℃ at last is incubated 2.5 hours down, makes its slow cool to room temperature in 8 hours.The block of preparation is taken out the back ball milling in reactor, powder sieving is become-300 purpose grades, obtain Ga
2Se
3Powder.Powder purity is greater than 99.95%.
The powder of preparing is put into diameter 350mm mould at the target that is processed into diameter 310mm under 600 ℃, 120MPa condition after with the hot-pressed sintering furnace compacting.The target density can reach 99.1%.
Embodiment 8
With Ga piece, the Se piece of purity 99.995%, behind Ga:Se=2:3.2 proportioning 400g, put into the autoclave of liner aluminium oxide ceramics, in molar ratio 7 * 10
-3Seal autoclave under the Pa vacuum degree condition.
It is gradient increased temperature constant temperature that autoclave is placed in the stove, promptly with the heating rate of 19 ℃/min, be divided into 5 sections intensification constant temperature for 1100 ℃ according to adjusting to the temperature that is higher than material melting point at last, the temperature of each temperature section is :-3 ℃+temperature/5+1 that is higher than material melting point that adjusts at last, promptly 5 sections thermostat temperatures are respectively 180 ℃, 360 ℃, 540 ℃, 720 ℃, 900 ℃, constant temperature time was respectively 2.5 hours, end temperature is adjusted to 1100 ℃ down insulation 8 hours of temperature conditions, makes its slow cool to room temperature in 8 hours.The block of preparation is taken out the back ball milling in autoclave, powder sieving is become-400 purpose grades, obtain Ga
2Se
3.2Powder.Powder purity is greater than 99.99%.
The powder of preparing is put into diameter 80mm mould at the target that is processed into diameter 75mm under 700 ℃, 150MPa condition after with the hot-pressed sintering furnace compacting.The target density can reach 99.3%.
As a kind of conversion of various embodiments of the present invention, when needed product was powder, cancellation hot-pressed sintering furnace pressing step got final product.
As a kind of conversion of the embodiment of the invention 2, embodiment 4 and embodiment 7, the described gas that charges in the closed container can also be helium.
As a kind of conversion of various embodiments of the present invention, described hot pressing furnace can also adopt the high temperature insostatic pressing (HIP) stove.
Above-described embodiment is preferable embodiments more of the present invention, and those skilled in the art can make various modifications within the scope of the appended claims.
Claims (10)
1. selenide material for absorbing layer of thin film solar cell preparation method, described selenide material is Cu
2Se
x, M
2Se
y, wherein M for or be selected from a kind of element among Al, In, the Ga, the value of x is 0.95～1.05, the value of y is 2.8～3.2, it is characterized in that: the preparation of above-mentioned selenide material may further comprise the steps:
A. required element material is put into container after by material composition requirement proportioning, less than 10
-2Under the Pa vacuum degree condition closed container or under the condition that charges into the argon gas, nitrogen or the helium that are lower than atmospheric pressure closed container;
B. airtight container is placed and be gradient increased temperature constant temperature in the stove, promptly with the heating rate of 10～20 ℃/min, be divided into 4～5 sections intensification constant temperature according to the temperature of adjusting at last that is higher than material melting point, each temperature section temperature is: the temperature that is higher than material melting point/(4～5)+1 of (30～+ 30) ℃+adjust at last, constant temperature time was respectively 2～4 hours, end temperature is adjusted under the temperature that is higher than material melting point and is incubated 0.1 hour～10 hours, make its slow cool to room temperature in 8 hours, the block of preparation is taken out the back ball milling in container, with powder sieving, obtain powder-product;
C. the powder of preparing is put into hot pressing furnace mould on demand dimensioned after 500 ℃～900 ℃, 30MPa～300MPa compacting and promptly obtained required block target.
2. the preparation method of selenide material for absorbing layer of thin film solar cell according to claim 1, it is characterized in that: the required element material described in the steps A is Cu and Se, and both mol ratios are: Cu: Se=2: 0.95～1.05.
3. the preparation method of selenide material for absorbing layer of thin film solar cell according to claim 1, it is characterized in that: the required element material described in the steps A is M and Se, and both mol ratios are: M: Se=2: 2.8～3.2.
4. according to the preparation method of claim 1,2 or 3 described selenide material for absorbing layer of thin film solar cell, it is characterized in that: the stove described in the step B is the nitrogen circulation cooling, and the furnace wall also has the stove of recirculated water cooling.
5. the preparation method of selenide material for absorbing layer of thin film solar cell according to claim 4 is characterized in that: when needed product is powder, and cancellation step C.
6. according to the preparation method of claim 1,2 or 3 described selenide material for absorbing layer of thin film solar cell, it is characterized in that: the temperature that is higher than material melting point described in the step B is 900 ℃～1250 ℃.
7. the preparation method of selenide material for absorbing layer of thin film solar cell according to claim 4, it is characterized in that: the temperature that is higher than material melting point described in the step B is 900 ℃～1250 ℃.
8. the preparation method of selenide material for absorbing layer of thin film solar cell according to claim 5, it is characterized in that: the temperature that is higher than material melting point described in the step B is 900 ℃～1250 ℃.
9. according to the preparation method of claim 1,2 or 3 described selenide material for absorbing layer of thin film solar cell, it is characterized in that: the container described in the steps A is autoclave, pressure pan, reactor or the retort of liner aluminium oxide ceramics, zirconia ceramics or enamel.
10. according to the preparation method of claim 1,2 or 3 described selenide material for absorbing layer of thin film solar cell, it is characterized in that: the hot pressing furnace described in the step C is high temperature insostatic pressing (HIP) stove or hot-pressed sintering furnace.
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| CN103526061B (en) * | 2013-08-01 | 2015-07-01 | 华南师范大学 | Regulation and control method for relative orientation of levels in layered microstructure of pyroelectric material |
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