前苏联专利SU1085510A3 Method and apparatus for producing composite film

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专利摘要:
A method and an apparatus are provided for performing growth of compound thin films by alternately repeating separate surface reactions of the substances comprising the compound. A carrier gas affects a diffusion barrier between the surface reaction steps to be separated from each other. The gas phase diffusion barrier is also applied to separate the source regions (12) of different reacting vapors both from each other and from the surface reaction zone.
公开号:SU1085510A3
申请号:SU802889600
申请日:1980-02-27
公开日:1984-04-07
发明作者:Сунтола Туомо；Паккала Арто；Линдфорс Свен
申请人:Ой Лохья Аб (Фирма)；
IPC主号:

专利说明:

2. A device for producing a film of various elements with a coke, including a reaction chamber connected to a vacuum system, a substrate holder mounted inside it, sources of vapors of substances connected to the reaction chamber and provided with a means of correlating the vapor supply, and it is provided with an inert separating gas source connected to the reaction chamber.
3. The device according to claim 2, characterized in that the sources of the vapors of the substances are connected to the reaction chamber by a tube, to which
an inert separating gas source is connected.
4. The PS device of Section 3, characterized in that the source of inert separating gas is connected to the tube by means of a pulse valve,
5. The device according to claim 2, characterized in that the reaction chamber is made in the form of sections that are connected at one end
with the vacuum system, and on the other alternately connected to the sources of vapor of substances and the source of inert separating gas, and the substrate holder is mounted rotatably and is made in the form of a paddle wheel.
The invention relates to methods for producing composite films of various types; composition and apparatus for carrying out this method.
The closest to the proposed method is the method according to which the process is carried out in an evacuated chamber by alternately contacting the substrate with vapors of substances containing various elements at a partial pressure ensuring the formation of one atomic layer per cycle. An apparatus for carrying out this method includes a reaction chamber connected to a vacuum system, a substrate holder mounted inside it, sources of material vapors connected to the reaction chamber and provided with a means to control the vapor supply, and heaters ij.
The disadvantages of the known method and device are the low purity of the layers obtained and the difficulty of controlling the process.
The purpose of the invention is to increase purity and improve process control.
This goal is achieved by the fact that according to the method of obtaining a composite film from different elements in an evacuated reaction chamber on the substrate surface, by alternately contacting with it vapors of substances containing these elements at their partial pressure, the academy will form one atomic layer in one cycle an inert separation gas is introduced into the reaction chamber.
Here, the device for producing a composite film of different elements, comprising a reaction chamber connected to a vacuum system, a holder for substrates installed inside it, sources of vapors of substances connected to the reaction chamber and provided with a means for controlling the supply of vapors, and heaters are supplied with an inert source. gas connected to the reaction chamber.
Preferably, the vapor sources of the substances are connected to the reaction chamber by a tube, to which a source of inert separating gas is connected.
In one embodiment, an inert separating gas source is connected to the pipe 1 with a pulse 0 valve.
In another embodiment, the reaction chamber is made in the form of sections that are connected at one end to the 5th vacuum system, and at the other end alternately connected to sources of vapor of substances and a source of inert separating gas, and the substrate holder is rotatably mounted and made in the form of a paddle wheel.
Figure 1 shows the pulses of chemically active vapor Ay and Bi and the diffusion barrier between them; Figure 2 shows the first version of the horizontal device, a section; in FIG. 3, section A-A in FIG. 2; in fig. 4 - eff-, the fact of self-stabilization of the growth rate, obtained with the proposed method, in comparison with the known; 0 in FIG. 5 - a typical magnetic field. pan, used as a source of pulses of chemically active gtar in accordance with the proposed method; Fig. 6 is an embodiment of a source of pulses of chemically active vapor in accordance with the proposed method; Fig. 7 is a simplified diagram of the circulation of the source of pulses in Fig. 6; in Fig. 8 is a vertical embodiment of the device, paspesj in Fig. 9 are sections BB, B-B and G-D in Fig. 8; FIG. 10 is a second variant of the horizontal device, a section; FIG. 11 - the same, top view; Fig. 12 shows an embodiment of a source of pulses that is intended for use in the device according to Fig. 11; 13 is a schematic diagram of an embodiment of devices for reciprocating movement of the substrates; on Fig - permit E-E on Fig; Fig. 15 is a schematic representation of the electroluminescence structure of a thin film created using the proposed method (according to example 4); in fig. 16 shows the measured brightness and light output curves characterizing the electroluminescent structure shown in FIG. 15; in fig. 17 shows the measured electrical properties of a thin film made according to Example 5. According to the invention, the pulses are different. chemically active vapors are sequentially directed to the substrate, causing the growth of the composite thin film. For example, such pulses of chemically active vapor (Fig. 1) AX and B at partial pressures PO between which there is a diffusion barrier are conducted through the reaction chamber, where the length of the diffusion barrier Xg in gas-medium C having velocity V during movement in the direction of x. The magnitude of the tg-duration of the diffusion barrier, which essentially interferes with the interaction of vapor substances, preventing any significant impact on the final product. The device for producing a composite film (.Frg.2) contains a glass reaction chamber 1, The main body of the structure, a source 2 with a tube 3 connecting the source with a reaction zone 4 located inside the chamber, a vacuum pump 5 with an outlet nozzle b extending from the chamber and serving to maintain neither pressure P and heater 7, is located nny around the region 4 of the reaction; The reaction zone through a port 8 at the end of the reaction chamber 1 is placed the substrate (or substrate) 9 .. The process of growing a thin film temperature of 10 podlozh1;: from the vile -rzhnnnyut using heating elements 11 regulated by adjusting standartnlsredstvom. g .. The pulses of chemically active vapors emanating from source 2 are controlled by a timing device and sequentially directed to the reaction zone according to the principle of EAS atomic beam epitaxy and the proposed method. The invention allows to obtain the effect of a self-stabilizing growth rate (pig. 4). Curve a shows the thickness profile of the thin film grown in accordance with the invention and with the aid of the device shown in FIG. 2. The thickness profile b is obtained as a result of the growth of the corresponding thin film, carried out by means of known means, when two reactive pairs must simultaneously react with the substrate. Two main types of devices are used to deliver pulses of chemically active vapor. The first is mechanical valves, which are known devices for supplying chemically active mg materials that have good volatility at room temperature (Fig. 5). Such valves include a nozzle 12, a housing 13, a solenoid 14 and a locking element 15, a valve hole 16 and an inert carrier gas supply nozzle 17 that communicate directly with the connecting pipe 3 coming from the source. The timing control 18 operates the valve. 6) the mechanical valve action is replaced by controlled diffusion barriers in the connecting tube between the source and the reaction chamber. This type of source is preferred in cases where the reactive material has a low vapor pressure and must therefore be directed to the reaction chamber at elevated temperature. Chemically active steam is produced by heating the chemically active material M in solid or liquid form in the source zone 19 with the help of a heating element 20. In the locked position, a diffusion barrier is formed in the source tube 21 with a carrier gas supplied from the connecting tube 22 and output through the connecting tube 23 to the suction pump 24. The corresponding diffusion barrier is also formed in the connection p; the source tube 3 to prevent diffusion of vapors in the reaction chamber to the source. In the locked position, the chemical vapor created in zone 19 is directed to condensation zone 25, where it can be cooled with the aid of cooling element 26. By controlling valve 27, the source from the locked position is transferred to the supply position in order to release additional carrier gas, the flow which is strong enough to deflect the direction of flow in the outlet tube 21 of the source.
A device for producing a composite film according to the second embodiment (Fig. 10) comprises a tubular reaction chamber, a source and a pumping means. The body of the reaction chamber 28 is made of stainless steel and is covered on the inside with glass plates 29; The pumping means includes a heating element 30, a condensation zone, 31, and a partition 32 for controlling the gas flow. Heater temperature controllers and a pulse source timing device are shown by blocks 33 and 34, respectively. In the pulse source (Fig. 12) intended for use in this device variant, the tubes 3.22 and 21 have a coaxial arrangement, formed by the output tube 21 of the source and glass tube 35. The outer source case 36 is made of stainless steel.
In both embodiments, the devices (Figs. 2 and 10) of the substrate in the reaction chamber in the process of growing a thin film are in a fixed position .. Chemically active pairs of pulses pass through the chamber and are moved by a carrier gas forming diffusion barriers between the pulses of chemically active vapor
Another method according to the invention involves the use of variants in which locally fixed flows of chemically active vapors separate one from another locally fixed flows of gases forming diffusion barriers. In such devices, a cyclic alternate interaction between the surface of the substrates and the reactive steam injected alternately with each stream is achieved by rotating or by another periodic mechanical movement of the substrates. From the point of view of the surface of the substrate, in both cases there is a similar situation in which the substrate is sequentially exposed to each reactive vapor in a gas-phase medium that separates the vapor by forming diffusion barriers between them.
Embodiments of devices involving the creation of locally fixed streams of chemically active vapors are shown in FIG. 8.9, 13 and 14. In the embodiment shown in FIG. 8 and 9, two sources 38 of chemically active vapors are placed in two opposite columns 39 and 37 of the housing 40 of the device. The sources are heated by heaters 41. Chemically active vapors are diffused or carried by carrier gases upwards, where they meet the substrate E, mounted in a rotating holder 42, forming a structure similar to the HfciiM blade wheel. When rotating the paddle impeller, each stream of reactive steam is alternately met when the latter passes through columns 39 and 37, respectively. Carrier gas flows from tubes 43 and 44 into columns 45 enter chemically active pairs in the space between the substrates as they pass through columns 45. In the channels enclosed between the substrates, the flow conditions of the flow are similar to the flow conditions shown in figure 10.
FIG. 8, means 46 for rotating the substrates, heater 47 is located opposite the reaction zone, between the vertical flow channels 39, 37 and 45 in FIG. 9A, corresponding to channels 39, 37, and 45 in FIG. 9B, walls 48 are located.
In the embodiment of the device shown in Figures 13 and 14, the interaction between the surface of the substrate and the chemically active pairs occurs due to the reciprocating movement of the substrate 9 over the stationary row of holes 49 of the source, holes 0 of the carrier gas and outlet openings 51. Diffusion barriers (Fig 14 is formed between the surface of the substrate and the body 52 containing a series of holes for the passage of gas flows. This device can be operated even at atmospheric pressure and without practically unprofitable high total velocity of the engine. carrier gas flow. 13 and 14 denote feeding carrier gas pipe 53, connecting pipes 54 source outlet tube 55 and springs 56 and 57 the reactive vapor.
Since the EAS-type process consists essentially of thousands of single steps of a surface reaction, providing thin film growth, the total ip of the process tends to be long, if you do not pay special attention to the minimal reduction in delays in the reaction cycles. In general, the quality factor E of the process of growing a thin film can be represented by the formula.,), (11 where T is the film thickness j the area of the substrate to be coated f tp is the duration of the process Ij is the loading and unloading time of the device. Device cost, power consumption and The efficiency of the source of materials n is taken into account. In an EAS type process, a thin film thickness can be expressed in the form, (2) where Tj, is the thickness obtained in one reaction cycle v W is the number of cycles. BO, Sz) where the time of one cycle to is the sum of impu periods There are various chemically active vapors t (, t2 ,, .., and intervals, D ;;.;, ... D; between them necessary to form diffusion barriers. In the case of a simple binary connection, AB iо looks like; to iAHiA4t6 t; e- I) The area A of the substrate to be processed during the process is determined by the size of the device and can vary over a wide range when using embodiments of the invention. The analysis of the work, which also includes the influence of the size of the device, is practically reduced to an analysis of the temporal indices i and 1 in the reaction cycle. The detailed analysis has been made with reference to the device variants shown in FIG. 2.3 10 and 11, in which the carrier gas flow moves with velocity V in a tubular reaction chamber having a free section A of the section, according to FIG. 1, where the total pressure P | and the partial pressure P of the pulses A X and Bij of reactive vapors are distributed along with the carrier gas flow in the x direction. Impulses of chemically active vapors tend to expand during propagation, due to diffusion in the carrier gas, as evidenced by the equation where G is the diffusion coefficient of chemically active vapor in the carrier gas. under the conditions of laminar flow in the reaction tube, if we neglect the effect of radial velocity profiles, equation (5) can be replaced by the diffusion equation in the x direction: IP nilP For simplicity, pressure P. Q along the edges of pulses is assumed to be constant during diffusion, obtained under boundary conditions. This assumption is also true for the calculation of the diffusion barrier formed in locally fixed locations, for example, in the source shown in FIG. 6 and 7, and in the embodiment shown in FIG. 14 and 13. The solution of equation 6 is the following P (), t) PoUB.O. (X), (7) where X is the distance from the edges of the pulse; i is the time from the moment of the pulse supply; i.VO.O. is the error probability interval. The pressure isobar is spread from the edges of the pulse in accordance with (8} where C means IVO, / Rd, Diffusion barrier, which has the ability to lower partial pressures A and By by the value of PB, has length X | ,, according to C8) Xg 2-Xpg 4 C-e-1 (OT. (10) At the speed V of the carrier gas, the length of the diffusion barrier x at the distance L from the point of impulse supply of chemically active vapors can be expressed as:, (11) that corresponds to the interval Ij, between the chemically active pulses defined by the formula; .ce / DLT r. (12) For practical calculations kozffitsient diffusion should be presented in the form. "out) where the constant value U does not depend on diffusion medium pressure ij, can be thus represented in the form of, ib 4-CE-fD --iL / vP. (14) According to equation (, 14) t, is highly dependent on the velocity V of the carrier gas, which can be expressed as V 5 / A, (15) where 5 is the pumping rate, A is the free section of the reaction tube. The use of a minimum amount of carrier gas for a certain value leads to a high amount at low pressure, which, however, cannot be lower than P. When determining the limits of the partial pressure of chemically active vapor Pd, one can proceed from the total atomic or molecular dose required to completely coat the surface of the substrate. According to the kinetic gas theory and the propagation geometry under consideration, the number of molecules of a chemically active gas per pulse can be expressed as.-V.te-PoAfkT, (16) where tg is the pulse duration. If the number of atoms necessary to form a complete coating per unit area of Nc, and the efficiency of using chemically active vapor C, the number of molecules required for a pulse of reactive vapor is determined by the formula h, - NsAs / n, tl7), where Ld is the area of the substrate. Cause n - “2 we get H 5As-kT about V-t, -A-n Equation (18), however, contains the measure of the pulse duration t for a given value of Pp. With a minimum value of i, P decreases. The upper limit of P is set by the carrier gas pressure, which is recognized as preferable for the minimum optimal flow, PjV and 1 conditions. Low flow rates are still beneficial for minimum radial pressure profiles P of reactive steam. Dp of a simple binary compound AB grown by the help of chemically active vapors A and Hz is the minimum value of the period of the IP process, determined by the formula (ii54i,), (19) which is obtained by doing i, and (A in the embodiments of the invention values for 1o are 0.1–1 and 0.05–0.5 s, respectively, with a total pressure P 0.5–5 mbar. When checking the analysis of one-dimensional diffusion, it can be seen that usually as pulse width V | i) and the width of the Xd-5 diffusion barriers is larger than the diameters of the reaction tubes, which can be considered as a criterion for a one-dimensional approach. In the given analysis of the fault, it was assumed that the impulses of chemically active vapors at the points of their supply have sharply rim edges. With the source shown in Fig. 5, this is easily achieved by using conventional valves. in the case of using the source shown in fig. b and 7, to obtain the desired situation it is necessary to carry out a detailed analysis. A locked source state is obtained when diffusion barriers are formed in tubes 43 and 12. Flow conditions in these tubes can serve as conditions for the formation of such diffusion barriers, by differentiating equation (8), which allows to determine the isobar velocity Vj in the carrier gas --SBL | 4Г 2СЬх 2СЕо р. (A diffusion barrier is created by the level i of the flow, which provides the velocity Vf V of the non-existing gas in x challah with area A / transverse .p2CeD / Xp (21) Then id 2Aj.ce (22) In the circulation diagram shown in Fig. 7, diffusion barriers in channels 43 and 12 can be determined: 2A2Ce D / U; jS (23 2 2A, C., (24) where A and A are the cross-sectional areas f L are the lengths of the channels, respectively 43 and 12. The condition for impulse input is receives the flow of carrier gas through valve 5, t1. The rise time of gas supply from the source is easily minimized compared to cig-H 1 ;, but some attention should be paid to the values of source volume C and conductivity (, c and c, in order to ensure a short delay at the moment of shutdown. Under normal conditions, the level f of the gas flow passing through the channel, be represented as fntPA-Pe), where P. and P "are the pressure at the end of the condensate constant, depending on the geometry of the channel and the properties of the given gas. Using equation (25) and the circulation diagram shown in Fig. 7, determine the pressure of the source R. as a function of the time that is flowing from the moment the valve is turned off: P.-Sl.P aECH-cw 5 where RNR is the pressure ix istochnikapri t 0v q (1 + ,,, / RIS / U-Pcco / PcoV; 2) Pcc.VP, p () r- z / ci + l, ™, Pressure P- (Fig.7) has the value ..) 32 Diffusion barrier in the tube at i2, CP7-Pc); (33). ivapV-poV (.go ti2. The rise time is a diffusion barrier, equal to the delay in the exit of impulses from a source, can be determined by formulas (34) and (26) and is MI-MS. (S ,,) g, /Pcc.C The safety limit for obtaining the minimum interval between two pulses of chemically active vapors can be ensured by adding the delay time of the pulse to the time t g. Analyzes made for the conditions of the formation of diffusion barriers in the gas phase medium would pi used in relation to the device variants shown in figs.2,3, 10 and 11. In addition, an analysis was made directly related to the case shown in figs 8 and 9 and easily modified to be applied to the case in fig 13 and 14. Example 1. The device variant shown in FIGS. 10 and 11 has the following parameters: reaction zone — DIN 40 cm, cross-sectional area of the main body, Ap 14–14 cm, free cross-section area, cm, speed of the suction pump, source (FIG. 12) - the volume of the cm hole of the source 0 0, cm, cm mbarS, the connecting pipe (12) 01.1-10 cm g, 8800 cm / mbar-s, the exhaust side section, 100 cm / mbar-s. Operational parameters (typical): pressure in the reaction zone, P. 2 mbar, pressure of the evacuation pump, 4 mbar, gas-phase medium flow (argon) of the source fo 5500 mbar-cm / s, pulse pressure at the source P 3 mbar. Using these parameters, we can, but calculate the following values: cm / mbar.s, 07 mbar,, 067, f 2 89 mbar-cm (with the corresponding ppm / p / p isobar at the center of the diffusion barrier), 0.030 , 05 s, if, 0.74 s. The safe time interval between pulses is approximately i, 0.8 s. The practice used the value of t; 1 sec. Example 2. Production of a thin film from the compound using the parameters defined in Example 1. Substrates (b): melted glass measuring 0.310 20 cm, temperature in the reaction zone, vaporous substances: Ta, CЙf from the source (Fig. 12) at 14 ° C ii 0.2 s; The NLO from the source shown in FIG. 5 1, () 0.2 s, T (HgO). Growing in 2500 cycles yields a thin film of Ta2Oc with a thickness of 1000 A on the substrates. Example 3. Production of thin films from p6 with an admixture of manganese Mn. A variant of the device according to example 1. Substrates, as in example 2, or preferably granulated glass 7059. The temperature in the reaction zone 450-C. Pairs of chemically active substances: 2pS2. MyiCe2 from sources in FIG. 12 at 380 and 510 ° C, respectively. Pulses of HPSE2 and MIS from sources are served simultaneously at t 0.2 s. From the source in Fig. 5, the sulfiding substance ti ,, t () is 0.2 seconds. Growing in 4500 cycles allows to obtain a film of ib (s) with a thickness of 4000 L on the substrates. Example 4. Ta2O5 + Xp5 (MI) thin films are made in accordance with examples 2 and 3 on glass substrates coated with a thin film of a conductive transparent layer of indium tin oxide, and the thin film is coated with a contact layer of aluminum, providing electroluminescent structure shown in Fig. The substrate 58 is covered with a transparent conductive layer of indium tin oxide 59, which in turn is covered with the first insulating layer 60 of, a film 61 of 2 pb (M), the second insulating layer 62 of and the aluminum electrode 63 allowing the electric field to be applied to the layered structure concluded between layers 59 and 63. At excitation of 2 kHz with a sinusoidal wave, the characteristics of luminance and light output of the structure are presented in FIG. Curve B shows brightness depending on the excitation voltage, and curve e shows the light output. Example 5. Making a film, the method is similar to the method in example 2, only TagSS replaces Ag C, at 9 5 C. The process, which includes 2800 cycles, makes it possible to obtain a thin film of a thickness of 2200 L at a temperature in the reaction zone 250 ° C, The electrical characteristics of the alumina film in a multilayer structure were measured, in which the APjO-j layer forms a plastic 2 / J ,, /, // / О ОО ОООООООООООБО | I KSKKK yy y (oooooQdyooQoT4 GZHT And fig. 2
tins capacitor between electrodes of aluminum thin film, having an active area of mm. FIG. Curve 17 shows the measured capacitance depending on the frequency, the curve is dielectric loss. M A-A
Phage.Z
(f) ut.8
g f,
Usr,
S /
29
20
nineteen
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yooooodoooooooo
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YuOOOO 5P
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/ 20 J5 22 "7 d
29
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i ::. o51es (ooo / o D 1
3

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权利要求:
Claims (5)
[1]
. METHOD FOR PRODUCING A COMPOSITE FILM AND A DEVICE FOR ITS IMPLEMENTATION 1. A method for producing a composite film from different elements in a vacuum reaction chamber on the surface of a substrate by alternately contacting with it vapor of substances containing these elements at their partial pressure, which ensures the formation of one atomic layer in one cycle, characterized in that, in order to improve purity and improve process control, after the deposition of each atomic layer, an inert separating gas is introduced into the reaction chamber.
THX
Phage one
108551 C
[2]
2. A device for producing an exiled film from various elements, including a reaction chamber connected to a vacuum system, a holder for substrates installed inside it, vapor sources of substances connected to the reaction chamber and provided with means for controlling the supply of vapors, and heaters, characterized in that it equipped with a source of inert separating gas connected to the reaction chamber.
[3]
3. The device according to claim 2, characterized in that the vapor sources of the substances are connected to the reaction chamber by a tube to which an inert separating gas source is connected.
[4]
4. The device according to claim 3, wherein the source of inert separating gas is connected to the tube using a pulse valve.
[5]
5. The device pop.2, characterized in that the reaction chamber is made in the form of sections / which are connected at one end to a vacuum system, and at the other end are connected alternately to sources of vapor of substances and an inert separating gas source, and the substrate holder is mounted for rotation and made in the form of a paddle wheel.

类似技术:

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同族专利:

公开号 | 公开日

NO800555L|1980-08-29|

EP0015390B1|1985-09-25|

IN152596B|1984-02-18|

PL222293A1|1980-11-03|

ZA80852B|1981-02-25|

PL138247B1|1986-08-30|

JPS6021955B2|1985-05-30|

AU5578680A|1980-09-04|

FI57975B|1980-07-31|

AU535151B2|1984-03-08|

AT15820T|1985-10-15|

HU181779B|1983-11-28|

US4413022A|1983-11-01|

CA1166937A|1984-05-08|

IL59393A|1983-06-15|

EP0015390A1|1980-09-17|

DK157943B|1990-03-05|

DK84680A|1980-08-29|

JPS55130896A|1980-10-11|

DK157943C|1990-08-27|

NO155106B|1986-11-03|

NO155106C|1987-02-11|

BR8001087A|1980-10-29|

DE3071110D1|1985-10-31|

MX151518A|1984-12-10|

FI57975C|1980-11-10|

IL59393D0|1980-05-30|

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FI790680A|FI57975C|1979-02-28|1979-02-28|OVER ANCHORING VIDEO UPDATE FOR AVAILABILITY|

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