CN1794424A - Solution method metal induced large grain polycrystalline silicon film material and its preparation and application - Google Patents
Solution method metal induced large grain polycrystalline silicon film material and its preparation and application Download PDFInfo
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Abstract
This invention relates to a large crystal grain polysilicon film material induced by metals with a solution method, its preparation and application, which takes noncrystalline silicon as the initial material to be induced by a solution stained with metal ions to generate a great crystal grain polysilicon, dissolves salt or alkali in alcohol, water or other solutions and an uniformed solution film is formed on the surface of noncrystalline silicon film after it is taken out from the solution to be dried by throwing, naturally or baked in an oven at 100deg.C or to be heated in a temperature quickly crystallizing or dissolving salt to oxide to be annealed under 400-600deg.C, which first of all forms crystallized inducing point in the process to be radiated laterally with the point as the center to be induced to a polysilicon at the 10-200 mum.
Description
Technical field
The present invention relates to the technology of preparing of polycrystalline silicon film material, particularly a kind of solution method metal induced large grain polycrystalline silicon film material and preparation and application.Utilize solution such as alcohol and a-Si and silicon oxide surface, the aqueous solution and silicon oxide surface that reasonable affinity is arranged, make the film surface that from nickel salt or nickel aqueous slkali, takes out to form the layer of even liquid film.Method forms equally distributed nickel silicon alloy, crystallization nickel salt or nickel oxide in amorphous silicon surfaces to adopt drying, natural air drying or toast etc. in baking oven, it is put into temperature is 400 ℃-600 ℃ annealing furnace annealing 4-10 hour, can obtain the polysilicon of crystallite dimension more than 10 micron dimensions.This method can be used for preparing technical fields such as polycrystalline SiTFT, SOI device or MEMS, has preparation technology and simplifies, pollutes little and characteristics such as cost is low.
Background technology
With metals such as nickel, aluminium, cobalts is the metal-induced crystallization technology of catalyst, what can significantly reduce solid phase phase transition temperature that amorphous silicon changes polysilicon into, employing because of it is batch process, and become one of competitive crystallization technology, have a wide range of applications in technical fields such as flat panel display, SOI.(Chinese patent 93114663.1, semiconductor device and manufacture method thereof).Amorphous silicon surfaces induce metal level can deposited by electron beam evaporation, method such as sputter, injection obtains, but the crystallite dimension of the polysilicon membrane that the annealing back obtains is smaller, and residual metals content is higher, with off-state current height, the on-off ratio of thin-film transistor (TFT) of preparation low, threshold voltage is high, anti-breakdown capability is poor, can't satisfy the application conditions in fields such as flat panel display; These methods that form metal induction layer all need to use vacuum equipment in addition, thereby preparation section relative complex, higher relatively (as: the Zhiguo Meng of preparation cost, Mingxiang Wang, and Man Wong, HighPerformance Low Temperature Metal-Induced Unilaterally Crystallized Polycrystalline SiliconThin Film Transistors for System-on-Panel Applications, IEEE TRANSACTIONS ONELECTRON DEVICES, VOL.47, NO.2, FEBRUARY 2000, p404-407).Another kind of method commonly used is exactly to form the layer of metal thin layer with solwution method by electroless-plating on amorphous silicon, need add solution such as NaOH during with this method, the pollution of Na ion will cause the decline even inefficacy (as: the Y-C CHEN of device performance, Y-C Sermon WU, C-W CHAO, G-R HU and M-S FENG, Electroless Plating Ni Induced Crystallization ofAmorphous Silicon Thin Films, Jpn.J.Appl.Phys., Vol.40 (2001), p5244-5246).Also have a kind of method be with Ni solution be spin-coated on first thermal annealing on the amorphous silicon membrane again laser annealing obtain to continue high-quality polysilicon (CGS) (as: the T Mizuki of growth, J-S Matsuda, Y Nakamura, J Takagi, and T Yoshida, LargeDomains of Continuous Grain Silicon on Glass Substrate for High-Performance TFTs, IEEETransactions on Electron Devices, Vol.51, p 204-211), the crystallite dimension of its optimization is greatly about 15 microns, but this method because adopt follow-up laser annealing not in that to have metal-induced crystallization technology simple, the advantage that equipment cost is low.
Summary of the invention
The purpose of this invention is to provide a kind of solution method metal induced large grain polycrystalline silicon film material and preparation and application.The present invention induces and produces the above polysilicon of 10 micron dimensions, and flow process is simple, is applicable to the crystallization method of the macromeritic polysilicon of large-scale production.The present invention is used to prepare technical fields such as polycrystalline SiTFT, SOI device or MEMS, has preparation technology and simplifies, pollutes little and characteristics such as cost is low.
Solution method metal induced large grain polycrystalline silicon film material provided by the invention, it is to form the metal inducement polysilicon on substrate, and described polysilicon is a large grain size polysilicon film, and crystal grain diameter is at the 10-200 micron.
The crystal grain diameter of described large grain size polysilicon film is 70 microns.
The preparation method of solution method metal induced large grain polycrystalline silicon film material of the present invention comprises the steps:
To contain the salt of catalytic metals such as comprising Ni, Au, Cu, Al, Pd, Co or Ag or corresponding alkali is water-soluble, in ammoniacal liquor, alcohol or other solvents; Large tracts of land is deposited on the amorphous silicon membrane on the substrates such as glass, quartz, monocrystalline silicon, stainless steel or plastics, dipping to concentration in this solution of 1ppm to 100000ppm, take out back drying, natural air drying or in 100 ℃ of baking ovens, dry, form equally distributed corresponding salt or alkali crystal on the surface of amorphous silicon membrane; Or place this kind salt or the alkali can rapid crystallization or be decomposed into the temperature heating of corresponding oxide the amorphous silicon membrane that dipping is crossed the salt that contains catalytic metal or aqueous slkali; Afterwards, through the nitrogen more than 400 ℃, vacuum or air atmosphere annealing, obtain the polysilicon of crystallite dimension (diameter) more than 10 micron dimensions.
The following step of preparation method's process of solution method metal induced large grain polycrystalline silicon film material of the present invention:
1) cryogenic oxidation silicon (LTO) or the silicon nitride of deposition 500nm on the large tracts of land substrate, or 300nm silicon nitride and 100nm LTO mixed layer are done transition zone, are used for stoping the metal impurities in the substrate to spread to active layer; Adopt PECVD, LPCVD, HW-CVD or sputtering method, on substrate, form the amorphous silicon membrane of large-area 30-200nm;
2) be dissolved in alcohol, water or the ammoniacal liquor with soluble nickel salt, nickel hydroxide, compound concentration is the nickel salt solution of 1-10000ppm;
3) the described amorphous silicon membrane of step 1) is dipped in the above-mentioned solution that contains nickel 10 seconds to 60 minutes, carries out chemical plating, take out back drying, natural air drying or in 100 ℃ of baking ovens, dry; Or place the nickel salt can rapid crystallization or be decomposed under the temperature of oxide and heat the amorphous silicon membrane that dipping is crossed nickel salt; Thereby form equally distributed crystallization nickel salt or nickel oxide in amorphous silicon surfaces;
4) putting into temperature is 400 ℃-600 ℃ annealing furnace, at N
2, annealing 2-10 hour in vacuum or the air atmosphere;
5) with sour pollutant or the residue that cleans up at silicon film surface;
6) remove surperficial natural oxidizing layer with hydrofluoric acid, can obtain the polysilicon of crystallite dimension more than 10 micron dimensions;
Described large tracts of land substrate is glass, quartz, monocrystalline silicon, stainless steel or plastics.
Described soluble nickel salt is nickel nitrate, nickel acetate, nickel phosphate, nickelous hypophosphite, nickel chloride or nickel iodide, or their mixing of two kinds.
Described acid is hydrochloric acid, hydrofluoric acid, phosphoric acid, nitric acid or sulfuric acid.
Solution method metal induced large grain polycrystalline silicon film material is used for preparing the technical fields such as polysilicon gate in low-temperature polysilicon film transistor, semiconductor integrated circuit or the micro mechanical system (MEMs) of flat-panel display device.
The present invention utilizes solution such as alcohol and a-Si and silicon oxide surface, the aqueous solution and silicon oxide surface that reasonable affinity is arranged, and makes the film surface that takes out from solution can form the layer of even liquid film.And conventional dipping method, because amorphous silicon surfaces is hydrophobic, the Ni inducing layer that is evenly distributed that is not easy to form, the crystal particle dimension difference of the polysilicon that the revulsive crystallization of using obtains is very big, and the spatial distribution of corresponding multi-crystal TFT performance is also very inhomogeneous.Metal-induced crystallization of the present invention, utilizing between solution such as alcohol, ammoniacal liquor and amorphous silicon surfaces or the aqueous solution and the natural oxidizing layer has reasonable affinity, thereby can form the uniform liquid film of spatial distribution in amorphous silicon surfaces.
The present invention does not use the chemical material that can pollute the characteristic of semiconductor of polysilicon.Conventional dipping method need add pH value and adjust agent (as NaOH), promoter (as Ji Er Suan Na), misfit agent, stabilizer etc. in salting liquid, the introducing of these chemicals can cause the decline of polysilicon semiconductor performance.
What play among the present invention that crystallization induces source effect is to form a kind of material in equally distributed crystallization nickel salt, nickel oxide and the nickel, wherein mixture, and the mixture of three kinds of materials of two kinds of materials in amorphous silicon surfaces.At the equally distributed crystallization nickel salt of amorphous silicon surfaces or alkali, nickel oxide or nickel and the equally distributed nucleus of inducing of silicon interaction formation.Can control the density of inducing a little by control nickel salt solution concentration, drying speed, temperature-rise period, thus the size of the crystal grain of control revulsive crystallization.When inducing dot density low, behind the annealing temperature more than 400 ℃, can obtain crystallite dimension greater than 10 microns super large grained polysilicon film.
The present invention adopts measures such as alcohol, natural oxidizing layer, makes solution can stick to sample surfaces to be annealed equably, thereby obtains the polysilicon membrane of even grain size.Natural oxidizing layer can play the effect that reduces residual metals content in the polysilicon simultaneously, thereby can improve the performance with the prepared semiconductor device such as TFT of this polysilicon.
The present invention utilizes the wettability of solution and film surface treating that the crystallization sample surfaces adheres to uniform liquid film and obtains the needed source metal of metal-induced crystallization, this method induces the method for metal to compare with routine with preparations such as evaporation, sputters, it is simple to have technology, preparation cost reduces, crystallite dimension is big, and residual metals content is low.Compare with the solution of routine, the crystal grain of prepared polysilicon is more even.
Above-mentioned detailed description is relevant of the present invention specifying, and does not allly break away from the equivalence that spirit of the present invention does and implements or change, all belongs to context of the present invention.
Description of drawings
Fig. 1: the schematic cross-section for preparing barrier layer, amorphous silicon layer on the large-area glass substrate.
Fig. 2: the amorphous silicon layer surface that is deposited forms the schematic cross-section of natural oxidizing layer.
Fig. 3: the schematic cross-section that on amorphous silicon or its natural oxidizing layer, forms nickel salt or nickel aqueous slkali film.
Fig. 4: nickel salt, nickel oxide and illegal silicon effect formation crystallization are induced schematic top plan view a little.
Fig. 5: to induce a little is the schematic diagram that horizontal induced growth is carried out at the center.
Fig. 6: to induce a little is the microphoto that nucleus carries out horizontal induced growth.
Fig. 7: the intermediate point at yellow little dot center, center to edge, the Raman spectrum of edge among Fig. 6.
Fig. 8: solution is induced and is produced the microphoto of macromeritic polysilicon after the TMAH corrosion.
Embodiment
Details are as follows with reference to accompanying drawing in the present invention:
As shown in the figure, the present invention utilizes solution treating that the crystallization sample surfaces forms uniform liquid film and obtains the needed source metal of metal-induced crystallization, and it is simple to have technology, and preparation cost reduces, and crystallite dimension is big and evenly, residual metals content is low.
Shown in Figure 1 is that the backing material 101 for preparing polycrystalline silicon device is glass.For stopping that the impurity in the glass substrate spreads in the thermal process of preparation, deposition 500nm cryogenic oxidation silicon (LTO) 102 on glass substrate in active layer.Predecessor---the amorphous silicon membrane 103 of preparation polycrystalline silicon material on LTO mixing barrier layer 102.
Shown in Figure 2 is: after sample takes out from the preparation chamber, can form the thin natural oxidizing layer 104 of one deck on amorphous silicon 103 surfaces.
Shown in Figure 3 is: the amorphous silicon substrate immersion concentration that will have natural oxidizing layer 104 is in the nickel acetate alcoholic solution of 5000ppm, takes out the back and form the nickel acetate solution film 105 that is evenly distributed on natural oxidizing layer.
Shown in Figure 4 is: after the samples of amorphous silicon that has a nickel acetate solution film 105 dries with 1000 rpms speed, put into temperature and be 170 ℃ convection oven baking 10 minutes, put into temperature again and be 550 ℃ N
2Annealing is after 2 hours in the atmosphere, and the yellow dots will polysilicon that occurs discrete distribution in amorphous silicon membrane 103 is induced a little 106 schematic diagram;
Shown in Figure 5 is: at 550 ℃ N
2Annealing in the atmosphere, is the schematic diagram that radial horizontal induced growth polysilicon grain 107 is carried out at the center to induce a little 106;
Shown in Figure 6 is: actual amorphous silicon substrate is at 550 ℃ N
25 hours microphoto (the microscope multiplication factor is 1000) of annealing in the atmosphere.In annealing process along with the lengthening of annealing time, crystal grain to around radiation growth, collide mutually up to the grain boundary.
Shown in Figure 7 is: the intermediate point at the round dot center of crystallization, center to edge, the Raman spectrum of edge among Fig. 6, and at 520cm
-1Sharp-pointed characteristic peak is arranged near the wave number, illustrate that this yellow round dot partly is the polysilicon of crystallization.
Shown in Figure 8 is: the hydrochloric acid with 37% cleaned 1 hour, remove the pollutant or the residue on surface, removed the natural oxidizing layer on surface in 1 minute with 1% hydrofluoric acid corrosion, the microphoto of TMAH corrosion after 3 minutes with 25%, four photos (a, b among the figure, c, d) be the microphoto of four zoness of different of same sample, crystal grain diameter is 70 microns, and size is more even.
Concrete preparation method is:
1) on large tracts of land substrate 101, adopts the method for plasma chemical vapor deposition (PECVD), at the excessive layer 102 of 350 ℃ of deposit 500nm cryogenic oxidation silicons as glass substrate impurity barrier layer and backing material and silicon fiml material.Be used for stoping the metal impurities in the substrate to spread to active layer; Adopt LPCVD on substrate, to form 100nm amorphous silicon membrane 103; From preparing the amorphous silicon that chamber or boiler tube take out, the surface can form the natural oxidizing layer 104 about one deck 3nm.
2) nickel acetate is dissolved in alcohol, concentration is 5000ppm.
3) amorphous silicon membrane dipping 10 minutes in the nickel acetate alcoholic solution of above-mentioned 5000ppm takes out the rear surface and is stained with uniform liquid film 105.After the speed drying with 1000RPM, place 170 ℃ temperature to heat amorphous silicon membrane.
4) putting into temperature is 550 ℃ annealing furnace, at N
2Middle annealing about 10 hours; At first form at amorphous silicon and equally distributedly to induce a little 106; Inducing a little 106 to be the center, crystal grain to around the radiation cross growth form as yet crystal grain 107 in the collision; Along with the growth of annealing time, crystal grain collides until adjacent grain boundary mutually with 4～5 microns speed cross growths hourly.
5) with 37% salt acid soak 1 hour, clean up pollutant or residue at silicon film surface.
6) with 1% hydrofluoric acid corrosion 1 minute, remove the natural oxidizing layer on surface, can obtain the polysilicon of crystallite dimension more than 10 micron dimensions, for devices such as preparation TFT.
By control nickel salt solution concentration, dipping time, drying speed, temperature-rise period, can control the density of inducing a little, thus the size of control crystal grain.Prepare the polysilicon of crystallite dimension with the present invention at the 10-200 micron.Fig. 8 is that the polysilicon membrane of crystallite dimension about 70 microns of actual acquisition is through 25% TMAH[Tetramethylammonium hydroxide, (CH
3)
4NOH] microphoto of corrosion after 3 minutes.
Claims (8)
1, a kind of solution method metal induced large grain polycrystalline silicon film material, it is to form the metal inducement polysilicon on substrate, it is characterized in that described polysilicon is a large grain size polysilicon film, crystal grain diameter 10-200 micron.
2, solution method metal induced large grain polycrystalline silicon film material according to claim 1, the crystallite dimension that it is characterized in that described large grain size polysilicon film are 70 microns.
3, a kind of preparation method who prepares the described solution method metal induced large grain polycrystalline silicon film material of claim 1 is characterized in that the following step of its process:
To contain that the salt that comprises Ni, Au, Cu, Al, Pd, Co or Ag catalytic metal or corresponding alkali are water-soluble, in ammoniacal liquor, alcohol or other solvents, concentration is 1ppm to 100000ppm, large tracts of land is deposited on amorphous silicon membrane dipping on the substrates such as glass, quartz, monocrystalline silicon, stainless steel or plastics in this solution, take out back drying, natural air drying or in 100 ℃ of baking ovens, dry, form equally distributed corresponding salt or alkali crystal on the surface of amorphous silicon membrane; Or place this kind salt or the alkali can rapid crystallization or be decomposed into the temperature heating of corresponding oxide the amorphous silicon membrane that dipping is crossed the salt that contains catalytic metal or aqueous slkali; Afterwards, through the nitrogen more than 400 ℃, vacuum or air atmosphere annealing, obtain the polysilicon of crystal grain diameter more than 10 micron dimensions.
4, a kind of preparation method who prepares the described solution method metal induced large grain polycrystalline silicon film material of claim 1 is characterized in that the following step of its process:
1) cryogenic oxidation silicon (LTO) or the silicon nitride of deposition 500nm on the large tracts of land substrate, or 300nm silicon nitride and 100nm LTO mixed layer are done transition zone, are used for stoping the metal impurities in the substrate to spread to active layer; Adopt PECVD, LPCVD, HW-CVD or sputtering method, on substrate, form the amorphous silicon membrane of large-area 30-200nm;
2) be dissolved in alcohol, water or the ammoniacal liquor with soluble nickel salt, nickel hydroxide, compound concentration is the nickel salt solution of 1-10000ppm;
3) the described amorphous silicon membrane of step 1) is dipped in the above-mentioned solution that contains nickel 10 seconds to 60 minutes, carries out chemical plating, take out back drying, natural air drying or in 100 ℃ of baking ovens, dry; Or place the nickel salt can rapid crystallization or be decomposed under the temperature of oxide and heat the amorphous silicon membrane that dipping is crossed nickel salt; Thereby form equally distributed crystallization nickel salt, nickel oxide or nickel in amorphous silicon surfaces;
4) putting into temperature is 400 ℃-600 ℃ annealing furnace, and annealing is 2-10 hour in N2, vacuum or air atmosphere;
5) with sour pollutant or the residue that cleans up at silicon film surface;
6) remove surperficial natural oxidizing layer with hydrofluoric acid, get final product;
5, the preparation method of solution method metal induced large grain polycrystalline silicon film material according to claim 4 is characterized in that described large tracts of land substrate is glass, quartz, monocrystalline silicon, stainless steel or plastics.
6, the preparation method of solution method metal induced large grain polycrystalline silicon film material according to claim 4 is characterized in that described soluble nickel salt is nickel nitrate, nickel acetate, nickel phosphate, nickel chloride or nickel iodide, or their mixing of two kinds.
7, the preparation method of solution method metal induced large grain polycrystalline silicon film material according to claim 4 is characterized in that described acid is hydrochloric acid, hydrofluoric acid, phosphoric acid, nitric acid or sulfuric acid.
8, the application of the described solution method metal induced large grain polycrystalline silicon film material of claim 1 is characterized in that being used for preparing the polysilicon gate of low-temperature polysilicon film transistor, semiconductor integrated circuit or micro mechanical system (MEMs).
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