CN102770946A - Method for producing a polycrystalline silicon layer, and apparatus for forming a metal mixed layer for same - Google Patents
Method for producing a polycrystalline silicon layer, and apparatus for forming a metal mixed layer for same Download PDFInfo
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- CN102770946A CN102770946A CN2011800102300A CN201180010230A CN102770946A CN 102770946 A CN102770946 A CN 102770946A CN 2011800102300 A CN2011800102300 A CN 2011800102300A CN 201180010230 A CN201180010230 A CN 201180010230A CN 102770946 A CN102770946 A CN 102770946A
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- 229910052751 metal Inorganic materials 0.000 title claims abstract description 325
- 239000002184 metal Substances 0.000 title claims abstract description 325
- 229910021420 polycrystalline silicon Inorganic materials 0.000 title claims abstract description 45
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 30
- 229910021417 amorphous silicon Inorganic materials 0.000 claims abstract description 87
- 238000002425 crystallisation Methods 0.000 claims abstract description 50
- 230000008025 crystallization Effects 0.000 claims abstract description 47
- 239000000463 material Substances 0.000 claims description 333
- 239000007789 gas Substances 0.000 claims description 183
- 238000001704 evaporation Methods 0.000 claims description 57
- 230000008020 evaporation Effects 0.000 claims description 57
- 239000000758 substrate Substances 0.000 claims description 55
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- 238000003860 storage Methods 0.000 claims description 32
- 230000002411 adverse Effects 0.000 claims description 24
- 238000013459 approach Methods 0.000 claims description 21
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- 239000000126 substance Substances 0.000 claims description 17
- 230000009471 action Effects 0.000 claims description 14
- 239000012159 carrier gas Substances 0.000 claims description 14
- 238000007669 thermal treatment Methods 0.000 claims description 14
- 238000002309 gasification Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 6
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 6
- 238000009987 spinning Methods 0.000 claims description 6
- 238000001514 detection method Methods 0.000 claims description 5
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- 230000007423 decrease Effects 0.000 claims description 4
- 229910052737 gold Inorganic materials 0.000 claims description 2
- 238000003780 insertion Methods 0.000 claims description 2
- 230000037431 insertion Effects 0.000 claims description 2
- 229910052763 palladium Inorganic materials 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- 239000011149 active material Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 34
- 230000008569 process Effects 0.000 abstract description 8
- 239000003054 catalyst Substances 0.000 abstract description 4
- 238000000137 annealing Methods 0.000 abstract 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 29
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 description 19
- 238000009792 diffusion process Methods 0.000 description 16
- 238000005516 engineering process Methods 0.000 description 14
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- 238000005229 chemical vapour deposition Methods 0.000 description 11
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- 239000011521 glass Substances 0.000 description 6
- 238000005240 physical vapour deposition Methods 0.000 description 6
- 230000033228 biological regulation Effects 0.000 description 5
- 238000010926 purge Methods 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 150000002739 metals Chemical class 0.000 description 4
- XZWYZXLIPXDOLR-UHFFFAOYSA-N metformin Chemical compound CN(C)C(=N)NC(N)=N XZWYZXLIPXDOLR-UHFFFAOYSA-N 0.000 description 4
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
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- NQLVCAVEDIGMMW-UHFFFAOYSA-N cyclopenta-1,3-diene;cyclopentane;nickel Chemical compound [Ni].C=1C=C[CH-]C=1.[CH-]1[CH-][CH-][CH-][CH-]1 NQLVCAVEDIGMMW-UHFFFAOYSA-N 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 230000002950 deficient Effects 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- 239000001307 helium Substances 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
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- 238000004062 sedimentation Methods 0.000 description 2
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- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
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- 230000005764 inhibitory process Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
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- 229910052742 iron Inorganic materials 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
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Images
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
- H01L31/186—Particular post-treatment for the devices, e.g. annealing, impurity gettering, short-circuit elimination, recrystallisation
- H01L31/1872—Recrystallisation
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02518—Deposited layers
- H01L21/02521—Materials
- H01L21/02524—Group 14 semiconducting materials
- H01L21/02532—Silicon, silicon germanium, germanium
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02365—Forming inorganic semiconducting materials on a substrate
- H01L21/02656—Special treatments
- H01L21/02664—Aftertreatments
- H01L21/02667—Crystallisation or recrystallisation of non-monocrystalline semiconductor materials, e.g. regrowth
- H01L21/02672—Crystallisation or recrystallisation of non-monocrystalline semiconductor materials, e.g. regrowth using crystallisation enhancing elements
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
Disclosed is a method for producing a polycrystalline silicon layer. The method for producing a polycrystalline silicon layer (22) according to one embodiment of the present invention involves contacting an amorphous silicon layer (20) and a metal mixed layer (30) with each other, and performing a crystallization annealing process on the amorphous silicon layer (20) so as to produce the polycrystalline silicon layer (22). According to the present invention, provided is a method for producing a polycrystalline silicon layer, in which a smaller amount of metal catalyst is used and a crystallization temperature is lowered.
Description
Technical field
The metal mixed layer that the present invention relates to a kind of manufacturing approach of polysilicon layer and be used for it forms device.More particularly, when the present invention relates to utilize the metal-induced crystallization method, import manufacturing approach and the metal mixed layer that is used for it that the little metal catalyst also can reduce the polysilicon layer of crystallization temperature and form device the amorphous silicon layer crystallization.
Background technology
The thin-film transistor (TFT:Thin Film Transistor) that is used for LCD (LCD:Liquid Crystal Display), OLED (OLED:Organic Light Emitting Display) etc. roughly is divided into non-crystalline silicon tft and multi-crystal TFT.
The characteristic of TFT is used the electron mobility evaluation, and the electron mobility of non-crystalline silicon tft is about 1 ㎝
2/ Vs, the electron mobility of multi-crystal TFT is about 100 ㎝
2About/Vs, therefore, the preferred multi-crystal TFT that adopts among the high performance LCD.
When making multi-crystal TFT, key is the crystallization processes of amorphous silicon layer.Particularly, preferably reduce crystallization temperature, crystallization temperature is too high when making TFT then can not use low-melting glass substrate, thereby has the too high problem of TFT manufacturing cost.Consider the workability of this glass substrate, proposed to form fast at low temperatures the various technologies of polysilicon layer recently.
Summary of the invention
Wherein, Metal-induced crystallization (MIC:Metal Induced Crystallization) method is on amorphous silicon, to apply the method that metallic catalysts such as Ni, Cu, Al are induced crystallization at low temperatures; Though have the advantage of crystallization at low temperatures; But owing to comprise a large amount of metals in the active region, so the defective that exists leakage current significantly to increase.
Like this; Though thereby the MIC method has the advantage that the crystallization temperature that reduces amorphous silicon when making TFT can be used glass substrate; But also there is the defective that reduces the TFT characteristic because of metallic pollution, therefore, preferred a small amount of as far as possible situation decline low crystallization temperature that imports metallic catalyst.
To this; The present invention proposes in order to solve said prior art problems; Its purpose is; Provide a kind of when utilizing the metal-induced crystallization method that amorphous silicon layer is carried out crystallization, also can reduce when importing the little metal catalyst crystallization temperature, utilize the metal mixed layer to make the method for polysilicon layer.
In addition, the object of the invention is, provides a kind of when being formed for that amorphous silicon layer carried out the metal mixed layer of metal-induced crystallization, and the metal mixed layer that can accurately control the metal source gas of supply response chamber forms device.
According to the present invention, when utilizing the crystallizing amorphous silicon layer of metal-induced crystallization method, utilize the metal mixed layer, also can reduce crystallization temperature even import the little metal catalyst.
In addition, according to the present invention, when being formed for that amorphous silicon carried out the metal mixed layer of metal-induced crystallization, can accurately control the amount of the metal source gas of supply response chamber.
Description of drawings
Fig. 1 is expression is formed with amorphous silicon layer on substrate according to one embodiment of the invention a sketch map.
Fig. 2 is expression is formed with the metal mixed layer on amorphous silicon layer according to one embodiment of the invention a sketch map.
Fig. 3 representes according to one embodiment of the invention the sketch map of the metal mixed layer that metal concentration is conditioned.
Fig. 4 representes that amorphous silicon layer is converted to the sketch map of polysilicon layer according to one embodiment of the invention.
Fig. 5 representes that perhaps the upper and lower is formed with the sketch map of the non-mixed layer of metal according to top, the bottom of one embodiment of the invention at the metal mixed layer.
Fig. 6 is a sketch map of representing on the metal mixed layer, to be formed with according to another embodiment of the present invention amorphous silicon layer.
Fig. 7 is the structure chart that the metal mixed layer that relates to of expression one embodiment of the invention forms device.
Fig. 8 is the structure chart of the metal source gas supply unit that relates to of expression one embodiment of the invention.
Fig. 9 is the sketch map of an example of the source material storage part of the metal source gas supply unit that relates to of expression one embodiment of the invention.
Figure 10 is another routine sketch map of the source material storage part of the metal source gas supply unit that relates to of expression one embodiment of the invention.
Figure 11 is the exploded perspective view of structure of the source material supply unit of the metal source gas supply unit that relates to of expression one embodiment of the invention.
Figure 12 is the cut-away section stereogram of structure of the source material supply unit of the metal source gas supply unit that relates to of expression one embodiment of the invention.
Figure 13 is the material evaporation part, source of the metal source gas supply unit that relates to of expression one embodiment of the invention and the structure chart of source material discharge portion.
Figure 14 is the exploded perspective view of structure of material evaporation part, source and the source material discharge portion of the metal source gas supply unit that relates to of expression one embodiment of the invention.
Figure 15 is the cutaway view of structure of material evaporation part, source and the source material discharge portion of the metal source gas supply unit that relates to of expression one embodiment of the invention.
Figure 16 to Figure 19 is the sketch map of action of the source material supply unit of the metal source gas supply unit that relates to of expression one embodiment of the invention.
Figure 20 is the cutaway view of the structure of the source material supply unit that relates to of expression another embodiment of the present invention.
Figure 21 is the sketch map of the reflectance that changes of the wavelength of the polysilicon layer of the polysilicon layer manufacturing approach manufacturing that relates to according to one embodiment of the invention of expression.
Reference numeral:
10: substrate
20: amorphous silicon layer
22: polysilicon layer
30: the metal mixed layer
32: metal
34: matrix
40; 40a, 40b, 40c, 40d: the non-mixed layer of metal
A: reative cell
B: metal source gas supply unit
C: substrate source gas supply part
D: upper electrode
E: lower electrode
F: assist gas supply unit
200: source material storage part
210: the purge gas supply pipe
220: filter house
250: source material supply pipe
260: the second monitor windows
270: cooling unit
300: material evaporation part, source
310: source material heater
312: power line
314: temperature measuring set
344: air hose
364: air hose
400: source material discharge portion
410: source material carriage
420: the upset actuator
422: the first pneumatic tubes
424: the three transducers
430: source material keeping bucket
440: the three monitor windows
442: transparency window
450: gate valve
452: the gate main body
454: gate
460: cylinder
462: the second pneumatic tubes
500: source material supply unit
510: main body
520: platform is supplied with in rotation
530: filling part
540: demarcation strip
550: supply hole
560: first sensor
570: the second transducers
600: the carrier gas supply unit
610: air supply pipe
620: blast pipe
700: adverse current prevents gas supply part
Embodiment
In order to realize said purpose; The manufacturing approach of the polysilicon layer that one embodiment of the invention relate to is characterized in that, after making amorphous silicon layer and metal mixed layer (metal mixed layer) contacting; Said amorphous silicon layer is carried out metal-induced crystallization heat treatment, thereby make polysilicon layer.
In addition; In order to realize said purpose, the metal mixed layer that one embodiment of the invention relate to forms device, is formed for amorphous silicon layer is carried out the heat treated metal mixed layer of metal-induced crystallization (metal mixed layer); It comprises: reative cell, dispose substrate; The metal source gas supply unit is supplied with metal source gas to said reative cell; And matrix (matrix) source gas supply part, supply with substrate source gas to said reative cell; Wherein, said metal source gas supply unit comprises: source material storage part, storage source material; Material evaporation part, source is a source gas with said source gasification substance; The carrier gas supply unit is supplied with carrier gas; With source material supply unit, be located between said source material storage part and the material evaporation part, said source, be used to regulate the source amount of substance that is supplied to material evaporation part, said source.
After the detailed description relevant of the present invention stated, reference example illustrates the accompanying drawing that can realize specific embodiment of the present invention.Make those of ordinary skill in the art can realize these embodiment of detailed description of the present invention.Be interpreted as, do not repel each other though various embodiment of the present invention differs from one another.For example, in concrete shape, structure and the characteristic of an embodiment of this record, under the situation that does not exceed thought of the present invention and scope, can realize by other embodiment.In addition, it will be appreciated that for, the position or the configuration of the indivedual inscapes among each embodiment that is disclosed under the situation that does not exceed thought of the present invention and scope, can change.So, after the detailed description stated be not to be used for limiting, protection scope of the present invention should be as the criterion with the record of claims with whole technological thoughts in the equal scope of the record of its claims.In the accompanying drawing similarly Reference numeral be the many-sided identical or similar function of expression, length and area, thickness etc. are for the ease of representing its shape, also might exaggerate expression.
Below, realize the present invention easily in order to make under the present invention the those of ordinary skill of technical field, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings.
The manufacturing approach of polysilicon layer
In the present invention, amorphous silicon layer 20 is carried out crystallization and thermal treatment to amorphous silicon layer 20 after contacting with metal mixed layer 30, as the characteristics on constituting.In the way of contact of amorphous silicon layer 20 and metal mixed layer 30, as shown in Figure 3, metal mixed layer 30 is contacted with on the amorphous silicon layer 20, as shown in Figure 6, amorphous silicon layer 20 is contacted with on the metal mixed layer 30.But both of these case, the crystallization principle of amorphous silicon layer 20 are in fact all the same, so following situation that is contacted with on the amorphous silicon layer 20 to metal mixed layer 30 and carries out crystallization and thermal treatment describes.Though; Amorphous silicon layer 20 is contacted with on the metal mixed layer 30 and the situation of carrying out crystallization and thermal treatment does not describe; But be interpreted as, the metal mixed layer 30 of explanation was contacted with on the amorphous silicon layer 20 and carries out the method for crystallization and thermal treatment below this situation can be suitable for too.
Fig. 1 to Fig. 7 is the sketch map of the manufacturing approach of the polysilicon layer 22 that is used to explain that one embodiment of the invention relate to.
On substrate 10, be formed with the sketch map of amorphous silicon layer 20 shown in Fig. 1.
With reference to Fig. 1, on substrate 10, form amorphous silicon layer 20.
Utilize the process of plasma enhanced chemical vapor deposition method formation amorphous silicon layer 20 and the structure of plasma enhanced chemical vapor deposition unit to belong to known technology, so omit detailed description in this manual to it.
In addition, in the present invention, the thickness of the amorphous silicon layer 20 that forms on the substrate 10 does not specifically limit.Therefore, the purpose that is utilized according to the present invention, the thickness of amorphous silicon layer 20 can change to difference.
Fig. 2 is illustrated in the sketch map that is formed with metal mixed layer 30 on the amorphous silicon layer 20.
With reference to Fig. 2, on amorphous silicon layer 20, form metal mixed layer 30.At this, metal mixed layer 30 meant the layer that is dispersed with metal 32 in the base matter inside of continuous phase.
The metal 32 that is comprised in the metal mixed layer 30, after in the crystallization and thermal treatment technology stated, can make amorphous silicon layer 20 crystallization at low temperatures.The kind of these metals 32 does not specifically limit, but preferred perhaps its mixture of any among Ni, Al, Ti, Ag, Au, Co, Sb, Pd, the Cu.
The basic substance of metal mixed layer 30, be matrix (matrix) 34, can carry out after suppress the function of metal 32 in the crystallization and thermal treatment technology stated to amorphous silicon layer 20 diffusion inside.The kind of these matrix 34 does not specifically limit, preferably Si oxide (SiO for example
x) or silicon nitride (SiN for example
x) in any or comprise both sides' material (Si (ON) for example
x).
In order to form metal mixed layer 30; The physical vaporous deposition (PVD:Physical Vapor Deposition) as sputtering method (sputtering) can be utilized, but chemical vapour deposition technique (CVD:Chemical Vapor Deposition) can be preferably utilized.The reason of utilizing chemical vapour deposition technique like this is to regulate the thickness of metal mixed layer 30 or the distribution of metal 32 etc. easily.When utilizing chemical vapour deposition technique to form metal mixed layer 30, can utilize various materials as the source gas of the material that constitutes metal mixed layer 30, but preferred following material.
At first, when the metal 32 that is comprised in the metal mixed layer 30 is Ni, can utilize Ni (cp) as source gas
2(two (cyclopentadiene) nickel; Dicyclopentadienyl nickel) or Ni (dmamb)
2In (two dimethylaminos-2-methyl-2-butoxy nickel) any.In addition, the matrix that comprised in the metal mixed layer 30 34 is during for Si oxide, can utilize SiH as the source gas of silicon
4Gas can utilize O as the source gas of oxide
2Or N
2O gas.In addition, the matrix that comprised in the metal mixed layer 30 34 is during for silicon nitride, can utilize SiH as the source gas of silicon
4Gas can utilize N as the source gas of nitride
2Or NH
3Gas.
In various chemical vapour deposition techniques, particularly can utilize plasma enhanced chemical vapor deposition method (PECVD:Plasma Enhanced Chemical Vapor Deposition) to form metal mixed layer 30 of the present invention.As stated, utilize the plasma enhanced chemical vapor deposition method, have the advantage that under low relatively low temperature, can form metal mixed layer 30 rapidly.
Utilize the plasma enhanced chemical vapor deposition method to form the process of metal mixed layer 30 and the structure of the metal mixed layer formation device that is used for it, clearly understand through following explanation meeting with reference to Fig. 7 to 20.
On the other hand, the purpose that is utilized according to the present invention, the metal 32 in the metal mixed layer 30 can be adjusted to various concentration.More particularly, metal 32 concentration in the metal mixed layer 30 can be adjusted to high or low.In addition, metal 32 concentration in the metal mixed layer 30 also can be adjusted to evenly, also can be adjusted to the direction of growth increasing or decreasing along metal mixed layer 30.
Fig. 3 is the sketch map of the metal mixed layer 30a that be conditioned of expression metal 32a, 32b, 32c concentration, 30b, 30c.
(a) of Fig. 3 is the sketch map that expression metal 32a concentration is adjusted to even metal mixed layer 30a.In order to make the metal 32a concentration in the metal mixed layer 30a even, form metal mixed layer 30a during, the amount of the metal 32a source gas of supplying with through the metal gas supply unit 240 of Fig. 4 remains unchanged.
(b) of Fig. 3 is the sketch map that expression metal 32b concentration is adjusted to the metal mixed layer 30b that increases progressively along the direction of growth of metal mixed layer 30b.For the metal 32b concentration in the metal mixed layer 30b is increased progressively along the direction of growth of metal mixed layer 30b; Along with the formation progress of metal mixed layer 30b, the amount of the metal 32b source gas in the reative cell of the plasma enhanced chemical vapor deposition unit of can increasing supply.
(c) of Fig. 3 is the sketch map that expression metal 32c concentration is adjusted to the metal mixed layer 30c that successively decreases along the direction of growth of metal mixed layer 30c.Successively decrease along the direction of growth of metal mixed layer 30c in order to make the metal 32c concentration in the metal mixed layer 30c; Along with the formation progress of metal mixed layer 30c, can reduce the amount of the metal 32c source gas in the reative cell of supplying with plasma enhanced chemical vapor deposition unit.
On the other hand, in the present invention, the thickness of the metal mixed layer 30 that on amorphous silicon layer 20, forms does not specifically limit.Therefore, the purpose that is utilized according to the present invention, the thickness of metal mixed layer 30 can change to different-thickness.
Fig. 4 is the sketch map that expression amorphous silicon layer 20 is converted to polysilicon layer 22.
With reference to Fig. 4, amorphous silicon layer 20 is carried out crystallization and thermal treatment.Thus, as shown in Figure 6, the metal 32 of metal mixed layer 30 is diffused into the inside of amorphous silicon layer 20, thereby amorphous silicon layer 20 changes into polysilicon layer 22.
At this moment, preferred heat treatment temperature is between about 500 ℃ to 700 ℃.In addition, preferred heat-treating atmosphere is any or its mixed atmosphere in inert gas atmosphere, reducibility gas atmosphere, the oxidizing gas atmosphere.At this, can utilize Ar, N as inert gas
2Deng, can utilize H as reducibility gas
2, NH
3Deng, can utilize O as oxidizing gas
2, N
2O, H
2O, ozone etc.
The metal 32 of metal mixed layer 30 is diffused into the inside of amorphous silicon layer 20 as seed (seed), plays the effect that promotes crystallization at low temperatures.At this moment, can cause that metallic pollution reduces the characteristic of solar cell, promote crystallization inner the time effectively so preferably let a spot of metal 32 be diffused into amorphous silicon layer 20 thereby be diffused into the inner metals 32 of amorphous silicon layer 20.
According to the present invention, when carrying out crystallization and thermal treatment after amorphous silicon layer 20 contacts with metal mixed layer 30, can promote crystallization effectively when making a spot of metal 32 be diffused into amorphous silicon layer 20 inside.This is specified as follows.
Along with the carrying out of crystallization and thermal treatment, the metal 32 of metal mixed layer 30 (for example Ni) is to amorphous silicon layer 20 diffusions.The metal 32 of metal mixed layer 30 passes through the matrix 34 (SiO for example of metal mixed layer 30 when the inner directly diffusion of amorphous silicon layer 20
x) diffusion, but the matrix 34 of metal mixed layer 30 suppresses metal 32 diffusions.So, can utilize the inhibition diffusion effect of this matrix 34, the concentration of the metal of suitably regulating in the metal mixed layer 30 to be comprised 32 and distribution etc. then can be regulated the degree of metal 32 to amorphous silicon layer 20 diffusion inside.
At this, metal 32 is meant to amorphous silicon layer 20 diffusion inside, not only comprises the amount of adjusting to the metal 32 of amorphous silicon layer 20 diffusion inside, also comprises regulating the meaning of metal 32 in the path of amorphous silicon layer 20 diffusion inside.Like this; As stated; It is a small amount of can regulating metals 32 amounts that are diffused into amorphous silicon layer 20 inside through the concentration that reduces the metal 32 in the metal mixed layer 30; Also can perhaps regulate the path of metal 32 through metal 32 concentration adjustment in the metal mixed layer 30 are become evenly to amorphous silicon layer 20 diffusion inside along the direction of growth increasing or decreasing of metal mixed layer 30.
The result; Through being contacted with metal mixed layer 30, amorphous silicon layer 20 carries out crystallization and thermal treatment; Can regulate to the amount and the path of the metal 32 of amorphous silicon layer 20 diffusion inside, promote crystallization inner the time effectively so can make a spot of metal 32 be diffused into amorphous silicon layer 20.
Fig. 5 is that the top, bottom or the upper and lower that are illustrated in metal mixed layer 30 are formed with the non-mixed layer 40 of metal; The sketch map of 40a, 40b, 40c, 40d.
With reference to Fig. 5, can also be formed with the non-mixed layer 40a of the metal that contacts with metal mixed layer 30,40b, 40c, 40d.More particularly; Shown in Fig. 5 (a); Can form the non-mixed layer 40a of metal on the top of metal mixed layer 30, shown in Fig. 5 (b), also can form the non-mixed layer 40b of metal in the bottom of metal mixed layer 30; Shown in Fig. 5 (c), also can all form the non-mixed layer 40c of metal, 40d in the upper and lower of metal mixed layer 30.
At this, the non-mixed layer 40a of metal, 40b, 40c, 40d are meant metal 32 unmixing layers.The non-mixed layer 40a of metal, 40b, 40c, 40d are similar to the matrix 34 of metal mixed layer 30, carry out the function that suppresses metal 32 diffusions.In this sense, the non-mixed layer 40a of metal, 40b, 40c, 40d can be made up of matrix 34 same substance with metal mixed layer 30.For example, the non-mixed layer 40a of metal, 40b, 40c, 40d can be by Si oxide (SiO for example
x), silicon nitride (SiN for example
x) or comprise these material (Si (ON) for example
x) constitute.
In order to form the non-mixed layer 40a of metal, 40b, 40c, 40d; Can utilize the physical vaporous deposition (PVD:Physical Vapor Deposition) as sputtering method (sputtering), preferably utilize chemical vapour deposition technique (CVD:Chemical Vapor Deposition).Particularly, in various chemical vapour deposition techniques, can utilize plasma enhanced chemical vapor deposition method (PECVD:Plasma Enhanced Chemical Vapor Deposition).
When utilizing the plasma enhanced chemical vapor deposition method to form the non-mixed layer 40a of metal, 40b, 40c, 40d, metal mixed layer 30 can original position (in-situ) form in a reative cell with the non-mixed layer 40a of metal, 40b, 40c, 40d.For example, utilize plasma enhanced chemical vapor deposition unit by Ni and SiO
xForm by SiO on the metal mixed layer 30 that constitutes
xDuring the non-mixed layer 40a of the metal that constitutes, can on the amorphous silicon layer 20 in the reative cell, supply with Ni (cp)
2Gas, SiH
4Gas and O
2Thereby, form by Ni and SiO
xThe metal mixed layer 30 that constitutes continues to supply with SiH afterwards
4Gas and O
2Thereby, form by SiO
xThe non-mixed layer 40a of metal that constitutes.
Like this, together carry out the non-mixed layer 40a of metal, 40b, 40c, the 40d that suppresses metal 32 diffusion functions through the matrix 34 of further formation and metal mixed layer 30, can more effectively regulate amount and path to the metal 32 of amorphous silicon layer 20 diffusion inside.
The metal mixed layer forms device
Fig. 7 is that the metal mixed layer that expression one embodiment of the invention relate to forms schematic representation of apparatus.
In the present invention; On substrate 10, form metal mixed layer 30; Not only be meant in the semiconductor applications normally used at substrate 10 from the situation that forms the metal mixed layer on one's body, be also included within the situation that forms metal mixed layer 30 on the amorphous silicon layer 20 that forms on the substrate 10.
With reference to Fig. 7, the metal mixed layer that one embodiment of the invention relate to forms device and comprises reative cell A.Reative cell A inner space term of execution of technology is airtight by substance, and is provided at the space that forms metal mixed layer 30 on the substrate 10.These reative cells A can keep optimum process condition, can manufacture rectangle or round-shaped.
The metal mixed layer that one embodiment of the invention relate to forms device can comprise metal source gas supply unit B.Metal source gas supply unit B can carry out function from metal source gas to reative cell A that supply with.According to the metal species that is comprised in the metal mixed layer 30, metal source gas can use various metal source gas.As an example, when the metal that is comprised in the metal mixed layer 30 is Ni, can utilize Ni (cp) as metal source gas
2(two (cyclopentadiene) nickel; Dicyclopentadienyl nickel) or Ni (dmamb)
2In (two dimethylaminos-2-methyl-2-butoxy nickel) any.
As stated; Metal source gas supply unit B can comprise source material supply unit 500; In order accurately to control the amount of the metal source gas of supplying with; This source material supply unit 500 is located between source material storage part 200 and the material evaporation part, source 300, to regulate the source amount of substance of supplying with to material evaporation part, source 300.Below, specify these structures.
Reative cell A can be connected through metal source gas supply pipe B ' with metal source gas supply unit B.Metal source gas can move to reative cell A from metal source gas supply unit B through this metal source gas supply pipe B '.
Though not shown in Fig. 7, on metal source gas supply pipe B ', can be provided with heater.Heater remains on more than the set point of temperature temperature of the metal source gas that moves to reative cell A, thereby prevents as far as possible that metal source gas from solidifying and sticked to metal source gas and supply with on the B '.As long as can the metal source gas that move be remained on the set point of temperature, the structure of heater is not limited to ad hoc structure, can adopt known various heater on the metal source gas supply pipe 24 of the present invention.
The metal mixed layer that one embodiment of the invention relate to forms device can comprise substrate source gas supply part C.Substrate source gas supply part C carries out the function with gas supply response chamber, the source A of the matrix that is comprised in the metal mixed layer 30.
According to the kind of the matrix that is comprised in the metal mixed layer 30, substrate source gas can use each source gas.For example, the matrix that is comprised in the metal mixed layer 30 is Si oxide (SiO for example
x) time, can utilize SiH as substrate source gas
4Gas and O
2In addition, the matrix that is comprised in the metal mixed layer 30 is silicon nitride (SiN for example
x) time, can utilize SiH as substrate source gas
4Gas and N
2
Reative cell A can be connected through substrate source gas supply pipe C ' with substrate source gas supply part C.Substrate source gas can move to reative cell A from substrate source gas supply part C through this substrate source gas supply pipe C '.With metal source gas supply pipe B ' similarly, on substrate source gas supply pipe C ', can be provided with heater (not shown), this heater remains on more than the set point of temperature temperature of the substrate source gas that moves to reative cell A.
Though not shown in Fig. 7, metal mixed layer of the present invention forms device can also comprise substrate heater (not shown).Substrate heater can be carried out the function that substrate 10 is applied heat, so that on substrate 10, form metal mixed layer 30 smoothly.The preferable substrate heater can make the temperature of substrate 10 rise to 100 ℃ to 300 ℃ temperature and continue to keep this temperature.The kind of substrate heater does not specifically limit.As long as can apply (for example the heating wire material is the Halogen lamp LED or kanthal (kanthal) heater of tungsten) of heat, all can be used as substrate heater of the present invention and adopt substrate 10.
Metal mixed layer of the present invention forms device and can also comprise: be applied in the upper electrode D of power supply in order to produce plasma and be used for carrying the lower electrode E that puts substrate 10.
Metal mixed layer of the present invention forms device can also comprise assist gas supply unit F, and this assist gas supply unit F supplies with and helps the assist gas (argon (Ar), helium (He)) that keeps plasma electron density to be evenly distributed.In order to supply with assist gas, assist gas supply unit F can be connected with reative cell A through assist gas supply pipe F '.
Below, explain that the metal mixed layer that utilizes Fig. 7 forms device and on amorphous silicon layer 20, forms by Ni and SiO
xThe method of the metal mixed layer 30 that constitutes.
At first, Ni (cp)
2Gas supplies to reative cell A through metal source gas supply unit B.In addition, SiH
4Gas and O
2C supplies to reative cell A through the substrate source gas supply part.In addition, Ar gas supplies to reative cell A through assist gas supply unit F.Afterwards along with applying high frequency electric source to upper electrode D, free electron (not shown) travel to and fro between between upper electrode D and the lower electrode E and with the gas collisions that is supplied to, comprise Si ion, O thereby produce
2The plasma of ion and Ni ion.At this moment, substrate 10 surface temperatures can remain between 100 ℃ to 300 ℃ through substrate heater (not shown), and the plasma that produces is in the surface reaction of amorphous silicon layer 30, to form by Ni and SiO
xThe metal mixed layer 30 that constitutes.
On the other hand, utilize the metal mixed layer formation device of Fig. 7 not only can form metal mixed layer 30, also can original position (in-situ) form the non-mixed layer 40 of aforesaid metal.Below, explain according to one embodiment of the invention by Ni and SiO
xOriginal position forms by SiO on the metal mixed layer 30 that constitutes
xThe method of the non-mixed layer 40 of metal that constitutes.
At first, on the amorphous silicon layer 20 that in reative cell A, disposes, supply with Ni (cp) through metal source gas supply unit B
2Gas, supply with SiH through substrate source gas supply part C
4Gas and O
2, to form by Ni and SiO
xThe metal mixed layer 30 that constitutes.Afterwards, metal source gas supply unit B ends to supply with Ni (cp)
2Gas, and substrate source gas supply part C continues to supply with SiH
4Gas and O
2Thereby, form by SiO
xThe non-mixed layer 40 of metal that constitutes.
Metal mixed layer of the present invention forms the upper electrode D that device also can adopt nozzle type, in chamber A, supplies with the reacting gas that is used to form metal mixed layer 30, that is, and and metal source gas, substrate source gas and assist gas etc.For this reason, for example on upper electrode D, can also form a plurality of holes (not shown) of even injection reacting gas.Spray reacting gas through nozzle type, can on amorphous silicon layer 20, spray reacting gas more equably, its result can form even metal mixed layer 30 more.
When adopting the upper electrode D of shower nozzle mode; Metal mixed layer of the present invention forms device can also comprise reacting gas supply pipe (not shown); This reacting gas supply pipe is connected with metal source gas supply pipe B ', matrix gas supply pipe C ' and assist gas supply pipe F ', plays to make metal source gas, substrate source gas and the auxiliary gas flow channeling to upper electrode D.
Fig. 8 is the structure chart of the metal source gas supply unit B that relates to of expression one embodiment of the invention.
With reference to Fig. 8, the metal source gas supply unit B that one embodiment of the invention relate to can comprise that source material storage part 200, material evaporation part, source 300, source material discharge portion 400, source material supply unit 500, carrier gas supply unit 600 and adverse current prevent gas supply part 700.
Source material storage part 200, source material supply unit 500 and material evaporation part, source 300; Dispose from top to bottom through source material supply pipe 250, material storage part 200 supplies to source material supply unit 500 to the source material from the source, material supply unit 500 supplies to material evaporation part, source 300 from the source with the freely falling body mode.Remain in the source material of material evaporation part, source 300, discharge through source material discharge portion 400 with the freely falling body mode.
Fig. 9 is the sketch map of an example of expression source material storage part 200.
With reference to Fig. 9, source material storage part 200 is made up of the container with regulation internal capacity, can store the source material.The source material can be the source material of metal source gas, for example the Ni of solid state (cp)
2Preferably source material storage part 200 is made into firmly, to prevent that outside foreign matter from invading or inner source material flows out.The material of source material storage part 200 can comprise stainless steel.
On source material storage part 200, can be provided with purge gas supply pipe 210 from purge gas to source material storage part 200 that supply with.Supply with the purge gas that is used to keep source material storage part 200 internal atmospheres through purge gas supply pipe 210.
One side of material storage part 200 can be provided with first monitor window (not shown) that can observe source material storage part 200 inside in the source.Can with the naked eye confirm the source object quantity of source material storage part 200 inside and the formation of source state of matter through first monitor window.
With reference to Fig. 8, can be connected with valve V on the source material supply pipe 250 once more.Valve V ends from the source material storage part 200 to source material supply unit 500 supply source materials when metal source gas supply unit B is carried out maintenance activity, perhaps after quantitative source material is supplied with in material evaporation part, source 300, close source material supply pipe 250 fully with no longer to material evaporation part, source 300 supply source materials from source material supply unit 500.
Can be provided with second monitor window 260 on the source material supply pipe 250.Second monitor window 260 is located at the lower end of valve V, can confirm that the source material is through valve V supply source material supply unit 500.The material of second monitor window 260 can comprise quartz.
Be used to connect on the source material supply pipe 250 of source material supply unit 500 and material evaporation part, source 300 and can be provided with cooling unit 270.Cooling unit 270 prevents that the heat that material evaporation part, source 300 is applied in order to generate metal source gas is delivered to source material supply unit 500 through source material supply pipe 250.
Figure 10 is another routine sketch map of expression source material storage part 200.
With reference to Figure 10, the inboard of material storage part 200 disposes the filter house 220 with regulation width of mesh in the source.Preferred filter house 220 uses the mesh screen (mesh) with certain width of mesh.The material of filter house 220 can comprise iron or aluminium.Filter house 220 makes the material evaporation part, source 300 that from the source material that the outside is supplied with, has prescribed level, states after promptly supplying to less than the source material of mesh screen width of mesh.Filter house 220 is limited in the source material size of supplying with below the setting, thereby can prevent because source material supply pipe 250 phenomenon of blocking that the source material particle was stated after big or small inhomogeneous causing.In order to improve the filter effect of filter house 220, filter house 220 can dispose a plurality of, at this moment, can the width of mesh of each filter house be made and differs from one another.
Figure 11 and Figure 12 are the exploded perspective view and the cut-away section stereograms of structure of the source material supply unit 500 of the metal source gas supply unit B that relates to of expression one embodiment of the invention.
Source material supply unit 500 is regulated the source amount of substance that supplies to material evaporation part, source 300 through source material supply pipe 250.For example, source material supply unit 500 can be regulated the source amount of substance that supplies to material evaporation part, source 300, and is all even to guarantee when carrying out the formation technology of metal mixed layer 30 at every turn.
With reference to Figure 11 and Figure 12, source material supply unit 500 can comprise main body 510, rotation supply platform 520, filling part 530, demarcation strip 540 and supply hole 550.In addition, source material supply unit 500 can also comprise the first sensor 560 and second transducer 570.In addition, source material supply unit 500 can also comprise that adverse current prevents gas supply part 700.
The skeleton of main body 510 formation source material supply units 500 is provided with the inscape of source material supply unit 500.Main body 510 is connected in the pars intermedia of source material supply pipe 250.Main body 510 can form the cylindrical shape that inside has the regulation space.Preferred main body 510 is made firmly, can prevent that outside foreign matter from invading or inner source material flows out.The material of main body 510 can comprise stainless steel.
For the ease of keeping in repair and managing the inscape that is located at main body 510 inside, can be connected with lid 512 on the top of main body 510 with opening and closing.The material of lid 512 is identical with main body 510, can comprise stainless steel.At the connecting portion of lid 512, can dispose sealing (sealing) with O shape ring 514 with main body 510.In a side of main body 510, can be connected with a pair of cooling water pipe 502 that cooling water flow out of inflow that is used for cools body 510.On the top of main body 510, the adverse current of stating after can being connected with prevents gas supply part 700.The inside lower end of preferred main body 510 forms the cross sectional shape of inverted triangle, so that the source material is discharged to the outside of main body 510 easily.
Rotatably be provided with rotation in the inside of main body 510 and supply with platform 520.Rotation supply with platform 520 will be from the source material supply unit 200 source material that supplies to material evaporation part, source 300 be limited in a certain amount of.Rotation is supplied with platform 520 and is formed the disc-shape with specific thickness.The central shaft that platform 520 is supplied with in rotation is connected on the rotary actuator 522, along with platform 520 rotations are supplied with in the action rotation of rotary actuator 522.At this moment, platform 520 is supplied with in rotation can rotate arbitrary set angle, for example 90 degree.Rotary actuator 522 can be located at the outer upper of main body 510.Supply with platform 520 rotations for the ease of rotation,, can dispose the ring 516 of polytetrafluoroethylene (Teflon) material at the upside of rotation supply platform 520.
The assigned position of supplying with on the platform 520 in rotation is formed with filling part 530.Fill in the filling part 530 and take care of temporarily the source material of supplying with the freely falling body mode through source material supply pipe 250 is arranged.Filling part 530 forms the cylindrical space with prescribed volume.At this, the volume size of filling part 530 can be stored the source amount of substance that produces a required metal source gas of metal mixed layer formation technology.
As shown in the figure, the angular distance with 90 degree on rotation supply platform 520 is formed with two filling parts 530, but also can be with the angle more than it, the for example angular distance formation of 180 degree.In addition, filling part 530 also can change form quantity and distance according to user's needs, forms more than two like the angular distance with 90 degree, for example forms four etc.
The downside of supplying with platform 520 in rotation is provided with demarcation strip 540.Demarcation strip 540 is divided into the upper and lower with the inner space of main body 510.In addition, demarcation strip 540 control through after the supply hole 550 stated be filled into the supply of the source material of filling part 530.
At this moment, because the constant volume of filling part 530, the source object quantity that is filled to this filling part 530 is also constant, so according to rotating the swing circle of supplying with platform 520, supply with quantitative source material to material evaporation part, source 300.Its result; In the present invention; Be stored in that source materials in the source material storage part 200 are supplied with the filling part 530 of platform 520 through rotation successively and the supply hole 550 of demarcation strip 540 supplies to material evaporation part, source 300, at this moment, whenever rotation supply with platform 520 be positioned at specified period supply hole 550 directly over the time; Supply with the source material (that is the source material of ormal weight) of the amount that is equivalent to filling part 530 volumes to material evaporation part, source 300.
Be set at two though supply with the quantity of the filling part 530 that forms on the platform 520 in rotation, be not limited thereto, can change to difference according to the per hour quantity delivered of source material.At this moment; In order to increase the per hour quantity delivered of source material; Under the identical situation of the quantity of filling part 530, can shorten the swing circle that platform 520 is supplied with in rotation, also can increase the volume of filling part 530 in addition; For example increase the diameter or the height (that is, the thickness of platform 520 is supplied with in rotation) of filling part 530.In other words; In the present invention; Per hour be supplied to the source amount of substance of material evaporation part, source 300 through source material supply unit 500, can carry out various changes through swing circle, the quantity of filling part 530 and the volume of filling part 530 etc. that platform 520 is supplied with in the change rotation.
Can be connected with adverse current on main body 510 tops and prevent gas supply part 700.Adverse current prevents that gas supply part 700 is connected the top of main body 510.Prevent that through adverse current the adverse current that gas supply part 700 is supplied with from preventing gas, can make that main body 510 is inboard to keep the authorized pressure states, thereby prevent that material evaporation part 300 produces in the source metal source gas is to source material supply unit 500 adverse currents.In addition, prevent through adverse current that gas supply part 700 gas supplied from can discharge and remain in the inner source material of main body 510.Adverse current prevents that gas supply part 700 can be through the pipeline receiver gases identical with carrier gas supply unit 600.Prevent that to adverse current gas supply part 700 gas supplied from can be Ar.
Figure 13, Figure 14 and Figure 15 are the material evaporation part, source 300 of the metal source gas supply unit B that relates to of expression one embodiment of the invention and structure chart, exploded perspective view and the cutaway view of source material discharge portion 400.
The 300 pairs of source materials of being supplied with by source material storage part 200 in material evaporation part, source apply heat, thereby make the source gasification substance.Material evaporation part 300 is supplied to reative cell A by gasification with the form of metal source gas to the source material in the source.400 discharges of source material discharge portion are produced metal mixed layer 30 by gasification and form the source material that the required metal source gas of technologies still remains in material evaporation part, source 300 afterwards.
With reference to Figure 13, Figure 14 and Figure 15, material evaporation part, source 300 can be made up of the container with regulation internal capacity.The inside of material evaporation part 300 can be provided with source material heater 310 in the source, and this source material heater is used to produce source gasification substance institute calorific requirement.Source material heater 310 can produce heat and impose on the source material, so that be placed on the source gasification substance on the source material carriage 410.Source material heater 310 forms the circular pin shape with specific length.In order to improve the heats of source material heater 310, preferably heating is concentrated in the end of material heater 310, the end that promptly is contacted with the source material heater 310 of source material carriage 410 in the source.
Can be connected with the temperature measuring set 314 of power line 312 that supply power is used to produce heat and the heat that is used to measure generation on the source material heater 310.The preferred temperature measuring set 314 preferred thermocouples (thermocouple) that use.Thermocouple belongs to known inscape in the present technique field, so omit the structure of thermocouple and the detailed description of effect.
The end of source material heater 310 can closely be connected in source material carriage 410.About detailing the back that is connected of source material heater 310 and source material carriage 410.
Carrier gas supply unit 600 is used to supply with carrier gas, this carrier gas will be in the source metal source gas carrying that produces of material evaporation part 300 to reative cell 10.The air supply pipe 610 and the blast pipe 620 of carrier gas supply unit 600 can be connected in a side of material evaporation part, source 300.On air supply pipe 610 and blast pipe 620, can be provided with and be used for the valve that control gaseous moves.Can use inertia and make highly purified argon that metal source gas moves to reative cell A, helium, nitrogen etc. easily as carrier gas.
With reference to Figure 13 and Figure 14, source material discharge portion 400 can comprise source material carriage 410, upset actuator 420 and source material keeping bucket 430.In addition, source material discharge portion 400 can also comprise gate valve 450 and cylinder 460.
The bottom of material carriage 410 is formed with heater connecting axle 412 in the source.Heater connecting axle 412 forms the tubulose with specific length.Can insert source material heater 310 in the inboard of heater connecting axle 412.The central shaft of preferred heater connecting axle 412 with after the central shaft of rotating shaft of the upset actuator 420 stated be positioned at coaxial on.In heater connecting axle 412 during the material heater 310 of insertion source, break away from and move about etc. in order to prevent source material heater 310, can dispose flange 316 and retainer ring 318.Source material carriage 410 can be formed by the metal material of easy transmission heat with heater connecting axle 412, can be formed by same material.
One side of material carriage 410 is connected with upset actuator 420 in the source.The upset actuator 420 source material carriage 410 that is used to overturn.For this reason, the rotating shaft of upset actuator 420 is connected with a side of source material carriage 410.For source material carriage 410 firmly is connected with upset actuator 420, can dispose mounting flange 426 and retainer ring 428.
Can be provided with a plurality of the 3rd transducers 424, so that detect the spinning movement of upset actuator 420.Preferred the 3rd transducer 424 is the angular distance setting of benchmark across 180 degree with the rotating shaft of upset actuator 420.The 3rd transducer 424 through with the rotating shaft that is located at upset actuator 420 on sensing element 425 contact and detects the whether Rotate 180 degree of actuator 420 that overturns.The 3rd transducer 424 can utilize fixed support to be fixed on a side of upset actuator 420.
Through the action of upset actuator 420, the upper face and the lower surface of source material carriage 410 can be overturn.When 410 upsets of source material carriage, be placed under the downward clan of source material on the source material carriage 410.
The bottom of material evaporation part 300 in the source disposes the source material of the source material that is used for the keeping discharge and takes care of bucket 430.The source material of keeping in source material keeping bucket 430 can reuse in after metal mixed layer 30 formation technology in, perhaps abandon fully.The preferred source material is taken care of the cylindrical shape that is shaped as of bucket 430, but is not limited thereto.
Material is taken care of a side of bucket 430 in the source, and the 3rd monitor window 440, the three monitor windows 440 that are formed with given size supply the source material of materials keeping bucket 430 inside, perusal source.Preferably in source material keeping bucket 430, dispose second transparency window 442, can separate the inside and outside of source material keeping bucket 430 through this second transparency window 442, and confirm the source material easily.The material of second transparency window 442 can comprise quartz.
Between material evaporation part, source 300 and source material keeping bucket 430, dispose the gate valve 450 that the source material that is used to control discharge moves.Gate valve 450 opens and closes with the action interlock of source material carriage 410.That is, when 410 upsets of source material carriage, gate valve 450 is open, so that the source material that material carriage 410 falls from the source passes through, when source material carriage 410 returned to original position, gate valve 450 cut out, and passed through to stop the source material.
Side at gate case 456 is connected with cylinder 460.The air pressure that cylinder 460 is supplied with through the outside makes gate valve 450 actions.On cylinder 460, be connected with a pair of second pneumatic tube 462.In a pair of second pneumatic tube 462, supply with air pressure to arbitrary second pneumatic tube, and discharge air pressure, thereby make cylinder 460 can carry out expanding-contracting action through another second pneumatic tube 462.Through changing the air pressure direction of the supply of pneumatic tube, can change the direction of action of cylinder 460, thereby change the moving direction of gate 454.
Preferred source material keeping bucket 430 and gate valve 450 encircle 432 with O shape and firmly are connected with fixed head 434 through sealing.
Below, the action of metal source gas supply unit B of the present invention is described with reference to Figure 11, Figure 12 and Figure 16 to Figure 19.
Figure 16 to Figure 19 is the sketch map of action of the source material supply unit 500 of the metal source gas supply unit B that relates to of expression one embodiment of the invention.At this, Figure 16 and Figure 17 are the sketch mapes of structure on the A direction of expression Figure 12, and Figure 18 and Figure 19 are the sketch mapes of representing the structure on the B direction of Figure 12.In Figure 16 to Figure 19, represent the source material as a reference with the part of shadow representation.
At first, the user opens the valve V that connects on the source material supply pipe 250, and the source material is moved through source material supply pipe 250 freely.
With reference to Figure 16, the source material that is stored in source material storage part 200 moves to source material supply unit 500 with the freely falling body mode through source material supply pipe 250.Afterwards, platforms 520 are supplied with in the 522 rotation rotations of the rotary actuator of source material supply unit 500 so that rotation supply with the filling part 530 of platform 520 be positioned at source material supply pipe 250 under.Thus, the source material of supplying with through source material supply pipe 250 moves to filling part 530, and is filled into filling part 530.Though the source material supplies to filling part 530 and fills, the lower end of filling part 530 is separated plate 540 closures, thereby can not discharge from the bottom.
After the source material is filled in the inboard of filling part 530, make rotation supply with platform 520 rotations through rotary actuator 522.Can know with reference to Figure 17, when platform 520 rotations are supplied with in rotation, under the filling part 530 disengaging source material supply pipes 250.
With reference to Figure 18, rotary actuator 522 makes rotation supply with the unspecified angle that platform 520 rotations are set, 90 degree for example so that filling part 530 be positioned at demarcation strip 540 supply hole 550 directly over.At this moment, whether first sensor 560 detection rotation supply platforms 520 rotate set angle.Be stored in the source material of filling part 530, the supply hole 550 through filling part 530 bottoms is supplied to material evaporation part, source 300.Whether second transducer, 570 detection resources materials fall through supply hole 550 and are provided.
On the other hand, in said process, material evaporation part 300 produces the source metal materials and when being provided, therefore the source metal material might be necessary to prevent this adverse current to source material supply unit 500 adverse currents in the source.In addition, supply with in order to carry out metal mixed layer 30 to form technology after the metal source gas,, need to remove the source material that remains in source material supply unit 500 for later metal mixed layer 30 forms technology.
For this reason, with reference to Figure 19, prevent that through adverse current gas supply part 700 supply adverse currents from preventing gas.That is, make filling part 530 be positioned at adverse current prevent gas supply part 700 under, supply with adverse current afterwards and prevent gas, the adverse current of then supplying with prevents that gas from supplying to main body 510 inside through filling part 530.Main body 510 inside prevent that through adverse current gas from keeping authorized pressure, thus can prevent metal source gas from the source material evaporation part 300 to source material supply unit 500 adverse currents.In addition, adverse current prevents that gas from can discharge the source material that remains in filling part 530.The source material of discharging moves to material evaporation part, source 300 through supply hole 550, thereby can remove the source material that remains in source material supply unit 500.
Through the source material of source material supply unit 500 weight feeds, be placed on the source material carriage 410 of 300 inboards, material evaporation part, source.
Afterwards; Operate source material heater 310; The heat that source material heater 310 is produced puts on the source material on the source material carriage 410, and then the source gasification substance becomes metal source gas, and supplies to reative cell A with the carrier gas of supplying with through air supply pipe 610 via blast pipe 620.
In addition, metal mixed layer 30 forms after the technology end, maybe the residual source material that ormal weight is arranged on source material carriage 410.
In order to discharge residual source material, supply with air pressure through first pneumatic tube 422 of upset actuator 420 1 sides, so that 420 actions of upset actuator.Through the spinning movement of upset actuator 420, the upset of the upper and lower of source material carriage 410, thus residual source material is fallen.At this moment, the 3rd transducer 424 detects whether Rotate 180 degree of upset actuator 420.
Afterwards, carry out the on-off action of gate valve 450 with the spinning movement interlock ground of upset actuator 420.That is, supply with air pressure to arbitrary first pneumatic tube 422 upset actuator 420 is overturn, arbitrary second pneumatic tube 462 that then is connected with cylinder 460 is also supplied with air pressure simultaneously.So when 410 upsets of source material carriage, gate 454 moves to the direction of opening gate main body 452, thereby the source material that falls from source material carriage 410 is moved in the source material keeping bucket 430 easily.
Make after the source material falls through upset source material carriage 41, supply with reverse air pressure through first pneumatic tube 422 of upset actuator 420, then source material carriage 410 returns to previous status.At this moment, second pneumatic tube 462 of cylinder 460 also is provided reverse air pressure, and gate 454 moves to the direction of closed shutter main body 452, to close the path to source material keeping bucket 430.
The source material that falls is taken care of in source material keeping bucket 430.The operator can pass through the 3rd monitor window 440 detection resources amount of substances, and the source material of keeping in source material keeping bucket 430, the metal mixed layer 30 after can being used in forms in the technology, perhaps abandons fully.
Figure 20 is the cutaway view of the structure of the source material supply unit 500 that relates to of expression another embodiment of the present invention.Source material supply unit 500 is that benchmark constitutes symmetrically with the central shaft, and for the ease of grasping the structure of source material supply unit 500, only illustrating in the drawings with the central shaft is a side of benchmark.
With reference to Figure 20, supply with the top of platform 420 in rotation, can form and have dispersing of specified altitude and prevent flange 580.Disperse and prevent that flange 580 and rotation supply platform 520 from forming concentric circless.Filling part 530 is prevented between the flange 580 a plurality of dispersing, disperse around filling part 530 to prevent the source material that material supply pipe 250 is supplied with to filling part 530 from the source.Prevent that being formed with between flange 580 and the filling part 530 disperses and prevent groove 582 dispersing.Disperse and prevent that groove 582 from forming and have specified volume, is used for retaining the source material that is not dispersed temporarily.Therefore, disperse and prevent that flange 580 from preventing that with dispersing groove 582 from can prevent that the source material from dispersing around filling part 530 and influence the action of source material supply unit 500.The structure and the effect of the source material supply unit of Figure 20 prevent that except dispersing flange 580 from preventing the groove 582 that with dispersing other is identical with above-mentioned source material supply unit, and the Therefore, omited is to its detailed description.
As stated; Metal mixed layer of the present invention forms device and comprises the source material supply unit that is located between source material storage part and the material evaporation part, source and is used to regulate the source object quantity of supplying with to material evaporation part, source, thereby can accurately control the amount of the metal source gas of supply response chamber.Thus, when forming the metal mixed layer, can regulate metal concentration and distribution in the metal mixed layer according to operator's needs.
This means; When carrying out the crystallization and thermal treatment of amorphous silicon layer; Metal integral diffusion in the amorphous silicon layer can be regulated according to operator's intention, and the result can make more a spot of metal diffusing when amorphous silicon layer is inner, more effectively promote the amorphous silicon layer crystallization.
Figure 21 is the sketch map of the reflectance that changes of the wavelength of the polysilicon layer of the polysilicon layer manufacturing approach manufacturing that relates to according to one embodiment of the invention of expression.
Manufacture process with polysilicon layer that the reflectance of Figure 21 changes is following.At first, on glass substrate, form amorphous silicon layer.Afterwards, on glass substrate, formed Ni-SiO
xLayer, promptly metal is Ni and matrix is SiO
xThe metal mixed layer.Ni-SiO
xLayer utilizes aforesaid metal mixed layer of the present invention to form device and forms.At this moment, the source material of Ni uses Ni (cp)
2Powder is with Ni (cp)
2Powder is heated to 83 ℃, and supplies with the source gas of Ni to chamber, simultaneously respectively with the flow of 500ccm and 2500ccm to the chamber supply as SiO
xThe SiH of source gas
4/ N
2O gas, thus Ni-SiO formed
xLayer.When chamber is supplied with Ni source gas, use the Ar of 400ccm flow as carrier gas.Deposition pressure is 1Torr, and deposition power is 800watt, and depositing temperature is 200 ℃, and sedimentation time is 10 minutes, and thickness is 2500A.Afterwards, at Ni-SiO
xUtilize PECVD method commonly used to form amorphous silicon layer on the layer.At this moment, source gas uses SiH
4/ N
2O/H
2Gas, the flow of each gas are 500ccm, 2500ccm, 3000ccm.Deposition pressure is 1Torr, and deposition power is 800watt, and depositing temperature is 200 ℃, and sedimentation time is 2 minutes, and thickness is 500A.Afterwards, use heat-treatment furnace (furnace) commonly used to carry out crystallization and thermal treatment, the amorphous silicon layer crystallization is become polysilicon layer.Heat-treat condition be 650 ℃ following 1 hour, atmosphere is blanket of nitrogen.At last, measured reflectance variation in order to estimate crystallization degree (degree of crystallinity) according to the wavelength of polysilicon layer.
With reference to Figure 21, compare reflectance variation according to the wavelength of amorphous silicon (a-Si) and polysilicon (s-Si), can find to have excellent degree of crystallinity according to the polysilicon layer (p-Si) that aforesaid process conditions are made.Hence one can see that, makes the method for polysilicon layer through utilizing metal mixed layer of the present invention, also can form the excellent polysilicon layer of degree of crystallinity.
In addition; Polysilicon layer manufacturing approach of the present invention and the metal mixed layer that is used for it form device; Not only can be applied to comprise with LCD (LCD) or the organic lcd display (OLED) of polysilicon layer, in all semiconductors that also can be widely used in polysilicon layer is comprised as active layer (active layer), display, solar cell, electronic component etc. as the polycrystalline SiTFT (P-Si Thin Film Transistor) of active layer (active layer).
The aforesaid preferred illustrated embodiment of the present invention is illustrated, but is not limited to said embodiment, and in the scope that does not depart from aim of the present invention, the those of ordinary skill of affiliated technical field can carry out various distortion and change.These variation and change example are contained in the protection range of putting down in writing in the present invention and claims.
Claims (23)
1. the manufacturing approach of a polysilicon layer is characterized in that, after making amorphous silicon layer and the metal mixed layer contacting, said amorphous silicon layer is carried out metal-induced crystallization heat treatment, thereby makes polysilicon layer.
2. the manufacturing approach of a polysilicon layer is characterized in that, after making amorphous silicon layer and the metal mixed layer contacting, said amorphous silicon layer is carried out metal-induced crystallization heat treatment, thereby makes polysilicon layer,
Said manufacturing approach comprises the steps:
(a) step of formation amorphous silicon layer on substrate;
(b) step of formation metal mixed layer on said amorphous silicon layer; And
(c) said amorphous silicon layer is carried out the step of crystallization and thermal treatment.
3. the manufacturing approach of a polysilicon layer is characterized in that, after making amorphous silicon layer and the metal mixed layer contacting, said amorphous silicon layer is carried out metal-induced crystallization heat treatment, thereby makes polysilicon layer,
Said manufacturing approach comprises the steps:
(a) step of formation metal mixed layer on substrate;
(b) step of formation amorphous silicon layer on said metal mixed layer; And
(c) said amorphous silicon layer is carried out the step of crystallization and thermal treatment.
4. like the manufacturing approach of claim 2 or 3 described polysilicon layers, it is characterized in that,
The metal of said metal mixed layer comprise among Ni, Al, Ti, Ag, Au, Co, Sb, Pd, the Cu any or two or more.
5. like the manufacturing approach of claim 2 or 3 described polysilicon layers, it is characterized in that,
The matrix of said metal mixed layer is any or two kinds in Si oxide or the silicon nitride.
6. like the manufacturing approach of claim 2 or 3 described polysilicon layers, it is characterized in that,
In said (b) step, regulate the metal concentration that is comprised in the said metal mixed layer.
7. like the manufacturing approach of claim 2 or 3 described polysilicon layers, it is characterized in that,
In said metal mixed layer, metal concentration is even.
8. like the manufacturing approach of claim 2 or 3 described polysilicon layers, it is characterized in that,
In said metal mixed layer, metal concentration increases progressively or successively decreases along the direction of growth of said metal mixed layer.
9. like the manufacturing approach of claim 2 or 3 described polysilicon layers, it is characterized in that, also comprise the steps:
On the top of said metal mixed layer or bottom or upper and lower form the step of the non-mixed layer of metal.
10. the manufacturing approach of polysilicon layer as claimed in claim 9 is characterized in that,
The non-mixed layer of said metal is any or two kinds in Si oxide or the silicon nitride.
11. a metal mixed layer forms device, is formed for amorphous silicon layer is carried out the heat treated metal mixed layer of metal-induced crystallization, it is characterized in that, comprising:
Reative cell disposes substrate;
The metal source gas supply unit is supplied with metal source gas to said reative cell; And
The substrate source gas supply part is supplied with substrate source gas to said reative cell;
Wherein, said metal source gas supply unit comprises:
Source material storage part, storage source material;
Material evaporation part, source is a source gas with said source gasification substance;
The carrier gas supply unit is supplied with carrier gas; And
Source material supply unit is located between said source material storage part and the material evaporation part, said source, is used to regulate the source amount of substance that is supplied to material evaporation part, said source.
12. metal mixed layer as claimed in claim 11 forms device, it is characterized in that, also comprises:
Apply upper electrode that produces the required power supply of plasma and the lower electrode that is placed with said substrate.
13. metal mixed layer as claimed in claim 11 forms device, it is characterized in that,
Said reative cell is connected through the metal source gas supply pipe with said metal source gas supply unit, on said metal source gas supply pipe, is provided with heater.
14. metal mixed layer as claimed in claim 11 forms device, it is characterized in that,
Said metal source gas supply unit also comprises source material discharge portion, and this source material discharge portion discharges and remains in the said source material in the material evaporation part, said source.
15. metal mixed layer as claimed in claim 11 forms device, it is characterized in that said source material supply unit comprises:
Main body;
Platform is supplied with in rotation, rotatably is located at said body interior;
Filling part is formed on said rotation and supplies with on the platform;
Demarcation strip is about said body interior is separated into; And
Supply hole is formed on the said demarcation strip with said filling part accordingly;
In said filling part, fill the said source material of supplying with from the outside; Said rotation is supplied with platform rotation unspecified angle and when making said filling part be positioned at the top of said supply hole, is filled in said source material in the said filling part and falls via said supply hole and be supplied to material evaporation part, said source.
16. metal mixed layer as claimed in claim 15 forms device, it is characterized in that,
Said metal source gas supply unit comprises that also detecting said rotation supplies with the first sensor whether platform rotates.
17. metal mixed layer as claimed in claim 15 forms device, it is characterized in that,
Said metal source gas supply unit also comprises second the transducer whether said source of detection material falls.
18. metal mixed layer as claimed in claim 15 forms device, it is characterized in that,
Said metal source gas supply unit also comprises and prevents that source gas from preventing gas supply part from material evaporation part, said source to the adverse current of said source material supply unit adverse current.
19. metal mixed layer as claimed in claim 15 forms device, it is characterized in that,
Said supply hole and said source material supply pipe across unspecified angle apart from formation.
20. metal mixed layer as claimed in claim 14 forms device, it is characterized in that, said source material discharge portion comprises:
Source material carriage can be located at the inside of material evaporation part, said source with spinning upside down;
The upset actuator is connected with an end of said source material carriage; And
Source material keeping bucket, the said source material that keeping is discharged from material evaporation part, said source;
Through the action of said upset actuator, the upset of said source material carriage, thus the said source material on the material carriage of said source is moved in the said source material keeping bucket.
21. metal mixed layer as claimed in claim 20 forms device, it is characterized in that,
Said metal source gas supply unit also comprises the heater connecting axle of tubulose, and this heater connecting axle is formed on the material carriage of said source, and the active material heater of its inboard insertion;
The rotating shaft of said heater connecting axle and said upset actuator be configured in coaxial on.
22. metal mixed layer as claimed in claim 20 forms device, it is characterized in that,
Said metal source gas supply unit also comprises the 3rd the transducer whether said upset actuator of detection rotates.
23. metal mixed layer as claimed in claim 20 forms device, it is characterized in that said metal source gas supply unit also comprises:
Gate valve opens and closes with said source material carriage interlock ground; And
Cylinder is connected with said gate valve;
When said source material carriage overturns, the open said gate valve of said cylinder, thus discharge said source material.
Applications Claiming Priority (5)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR10-2010-0018211 | 2010-02-26 | ||
| KR1020100018211A KR101120045B1 (en) | 2010-02-26 | 2010-02-26 | Method for manufacturing poly crystalline silicon layer |
| KR10-2010-0033517 | 2010-04-12 | ||
| KR1020100033517A KR101129035B1 (en) | 2010-04-12 | 2010-04-12 | Apparatus for forming metal mixed layer |
| PCT/KR2011/001296 WO2011105830A2 (en) | 2010-02-26 | 2011-02-24 | Method for producing a polycrystalline silicon layer, and apparatus for forming a metal mixed layer for same |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102770946A true CN102770946A (en) | 2012-11-07 |
Family
ID=44507442
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011800102300A Pending CN102770946A (en) | 2010-02-26 | 2011-02-24 | Method for producing a polycrystalline silicon layer, and apparatus for forming a metal mixed layer for same |
Country Status (4)
| Country | Link |
|---|---|
| JP (1) | JP2013520832A (en) |
| CN (1) | CN102770946A (en) |
| TW (1) | TW201214523A (en) |
| WO (1) | WO2011105830A2 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104465319A (en) * | 2014-10-30 | 2015-03-25 | 深圳市华星光电技术有限公司 | Manufacturing method for low-temperature polycrystalline silicon and manufacturing method for TFT substrate |
| CN111312612A (en) * | 2018-12-11 | 2020-06-19 | 东芝存储器株式会社 | Substrate processing apparatus and substrate processing method |
| CN111312612B (en) * | 2018-12-11 | 2024-04-12 | 铠侠股份有限公司 | Substrate processing apparatus and substrate processing method |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105624645B (en) * | 2014-11-06 | 2018-04-24 | 中微半导体设备(上海)有限公司 | Reacting gas conveying device and chemical vapor deposition or outer layer growth reactor |
| KR101959754B1 (en) * | 2018-02-27 | 2019-03-19 | 한국과학기술원 | Forming method of sensing film for uncooled type infrared sensor, sensing film formed by the method, manufacturing method of uncooled type infrared sensor and uncooled type infrared sensor manufactured by the method |
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| KR20090016232A (en) * | 2007-08-10 | 2009-02-13 | 주성엔지니어링(주) | Plasma processing apparatus for film deposition and deposition method of micro crystalline silicon layer using the same |
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| WO2001057289A1 (en) * | 2000-02-04 | 2001-08-09 | Aixtron Ag | Device and method for depositing one or more layers onto a substrate |
| DE10212923A1 (en) * | 2002-03-22 | 2004-01-08 | Aixtron Ag | Process for coating a substrate and device for carrying out the process |
| KR100522436B1 (en) * | 2003-02-05 | 2005-10-20 | 장 진 | Fabrication method of polycrystalline silicon thin film transistor using a cap layer |
| KR100721555B1 (en) * | 2004-08-13 | 2007-05-23 | 삼성에스디아이 주식회사 | Bottom gate thin film transistor and method fabricating thereof |
| KR100929093B1 (en) * | 2007-12-26 | 2009-11-30 | 재단법인서울대학교산학협력재단 | Crystallization method of amorphous silicon thin film using metal induced vertical crystallization and manufacturing method of polycrystalline thin film transistor using same |
-
2011
- 2011-02-24 WO PCT/KR2011/001296 patent/WO2011105830A2/en active Application Filing
- 2011-02-24 JP JP2012554931A patent/JP2013520832A/en not_active Withdrawn
- 2011-02-24 CN CN2011800102300A patent/CN102770946A/en active Pending
- 2011-02-25 TW TW100106452A patent/TW201214523A/en unknown
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1133489A (en) * | 1994-10-20 | 1996-10-16 | 株式会社半导体能源研究所 | Method for making semiconductor device |
| US6033732A (en) * | 1994-12-28 | 2000-03-07 | Mitsushita Denki Kabushiki Kaisha | Apparatus for and method of forming thin film by chemical vapor deposition |
| KR20090016232A (en) * | 2007-08-10 | 2009-02-13 | 주성엔지니어링(주) | Plasma processing apparatus for film deposition and deposition method of micro crystalline silicon layer using the same |
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| CN104465319A (en) * | 2014-10-30 | 2015-03-25 | 深圳市华星光电技术有限公司 | Manufacturing method for low-temperature polycrystalline silicon and manufacturing method for TFT substrate |
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| CN111312612A (en) * | 2018-12-11 | 2020-06-19 | 东芝存储器株式会社 | Substrate processing apparatus and substrate processing method |
| CN111312612B (en) * | 2018-12-11 | 2024-04-12 | 铠侠股份有限公司 | Substrate processing apparatus and substrate processing method |
Also Published As
| Publication number | Publication date |
|---|---|
| TW201214523A (en) | 2012-04-01 |
| WO2011105830A3 (en) | 2012-02-09 |
| WO2011105830A2 (en) | 2011-09-01 |
| JP2013520832A (en) | 2013-06-06 |
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Application publication date: 20121107 |