Summary of the invention
The object of the invention is to the above-mentioned defect overcoming prior art existence, provide a kind of technique for atomic layer deposition to prepare the implementation method of film, to improve the utilization ratio of reaction source, reduce Processes and apparatus cost.
For achieving the above object, technical scheme of the present invention is as follows:
Technique for atomic layer deposition prepares an implementation method for film, comprises the following steps:
Step S1: the valve opening of giving vent to anger reducing reaction chamber, passes into the first reaction source, forms the process to reaction chamber inflation, reaction chamber pressure is raised gradually, to increase effective diffusion time of the first reaction source;
Step S2: valve of giving vent to anger is opened completely, and pass into sweeping gas and purge, the first reaction source residual in reaction chamber is extracted out;
Step S3: the valve opening of giving vent to anger reducing reaction chamber, passes into the second reaction source, forms the process to reaction chamber inflation, reaction chamber pressure is raised gradually, to increase effective diffusion time of the second reaction source;
Step S4: valve of giving vent to anger is opened completely, and pass into sweeping gas and purge, the second reaction source remained in reaction chamber is extracted out.
Preferably, step S1 comprises:
Step S11: the valve opening of giving vent to anger reducing reaction chamber, passes into the first reaction source;
Step S12: stop the first reaction source to pass into, and pass into diluent gas, forms the process to reaction chamber inflation, reaction chamber pressure is raised gradually, to increase effective diffusion time of the first reaction source.
Preferably, step S3 comprises:
Step S31: the valve opening of giving vent to anger reducing reaction chamber, passes into the second reaction source;
Step S32: stop the second reaction source to pass into, and pass into diluent gas, form the process to reaction chamber inflation, reaction chamber pressure is raised gradually, to increase effective diffusion time of the second reaction source.
Preferably, the valve opening of giving vent to anger of reaction chamber is decreased to zero, is namely in buttoned-up status.
Preferably, being formed in the process of reaction chamber inflation, the pressure of reaction chamber is made to be elevated to 0.5-10Torr gradually.
Preferably, the pressure of reaction chamber is made to be elevated to 1-5Torr gradually.
Preferably, described diluent gas adopts reaction source carrier gas or sweeping gas.
Preferably, described diluent gas is nitrogen or rare gas element.
As can be seen from technique scheme, the present invention proposes a kind of self-diffusion formula ALD technology, reaction chamber is utilized to give vent to anger the opening and closing of valve, control the diffusion of reaction source in reaction chamber, by carrying out reducing to give vent to anger valve opening or closed in technological process passing into reaction source, to increase pressure in reaction chamber, thus increase effective diffusion time of reaction source, and by passing into the diffusion that diluent gas promotes reaction source in technological cycle process, the utilization ratio of reaction source can be improved on the one hand, reduce process costs, also the requirement to reaction chamber pressure Controlling System can be reduced on the other hand, thus can equipment cost be reduced, meanwhile, because reaction source has the longer time can spread in reaction chamber, the homogeneity of prepared film can also be improved.
Embodiment
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is described in further detail.
Existing when carrying out ALD technique on time type ALD equipment, in ALD technological process, the outlet side of reaction chamber is in the state always having gas to flow out, and pressure in reaction chamber is maintained in certain numerical range by valve system.The shortcoming of this technological process is, one is the increase in the accuracy requirement to pressure control system, thus improves the production cost of equipment; In addition, due to reaction source gas continuous flow, cause having a large amount of reaction sources directly to be carried out reaction chamber, thus cause waste, also improve process costs to a certain extent.
For the problems referred to above, the present invention proposes the implementation method that a kind of self-diffusion formula ALD technology prepares film, reaction chamber is utilized to give vent to anger the opening and closing of valve, and by technological cycle process, to increase effective diffusion time of reaction source and to increase the mode of pressure in reaction chamber, control the diffusion of reaction source in reaction chamber.The method may be used for depositing multiple nano-level thin-membrane.
Core concept of the present invention is: carry out in technological process passing into reaction source, by reducing to give vent to anger valve opening, forming the process to reaction chamber inflation, reaction chamber pressure is raised gradually, thus increase effective diffusion time of reaction source, improve the utilization ratio of reaction source.
In following the specific embodiment of the present invention, be described for industrial comparatively conventional deposited aluminum oxide thin film.First refer to Fig. 1, Fig. 1 is the implementation method schema that a kind of technique for atomic layer deposition in one of better embodiment of the present invention one prepares film; Meanwhile, incorporated by reference to consulting Fig. 3, Fig. 3 is a kind of gas circuit distribution schematic diagram of ALD system.As shown in Figure 1, technique for atomic layer deposition of the present invention prepares the implementation method of film, can comprise following four stages:
In the stage one: the valve opening of giving vent to anger reducing reaction chamber, passes into the first reaction source, form the process to reaction chamber inflation, reaction chamber pressure is raised gradually, to increase effective diffusion time of the first reaction source.
Refer to Fig. 3.When ALD technique starts, first, close corresponding pneumavalve 4, comprise and the pneumavalve V1, the V8 that are located at diluent gas pipeline, pneumavalve V2, V4, V5 of being located at sweeping gas pipeline and the pneumavalve V6 being located at steam evaporator 2 pipeline, the pneumavalve V7 that is located at ozonizer 1 pipeline are closed; And the aperture being located at the pneumavalve V9 (valve of namely giving vent to anger) at reaction chamber venting port 6 place is reduced, such as the aperture of valve of giving vent to anger can be reduced to less than 1/3 of maximum opening.Then, open the pneumavalve V3 being located at gaseous state trimethyl aluminium producer 3 pipeline, in reaction chamber 5, pass into TMA (trimethyl aluminium) as the first reaction source.In the process, because the aperture of valve of giving vent to anger obviously reduces, make the output of gas be less than air input, thus form the process to reaction chamber inflation, and the pressure in reaction chamber is raised gradually; Like this, the diffusion time of TMA can be increased.Meanwhile, TMA compares the state that existing pressure remains unchanged within the scope of certain numerical value, can carry out self-diffusion better, thus improve the utilization ratio of TMA under being in the pressure state constantly raised.
According to different processing requirements, as an optional embodiment, the pressure in reaction chamber can be made in the process to be increased to 0.5-10Torr gradually, be preferably 1-5Torr.Can be regulated the pressure in reaction chamber by valve system, make it be in the scope of needs.By making the pressure in reaction chamber raise gradually, reduce the requirement to reaction chamber pressure Controlling System; Also because of the raising of TMA self-diffusion ability, TMA can be spread more fully in reaction chamber, the utilization ratio of TMA can be improved equally, and improve the homogeneity of prepared film.
As one preferred embodiment, when passing into TMA, the aperture of valve of giving vent to anger can be reduced to zero, even if show that air valve is closed completely, thus the pressure in reaction chamber can be increased the most rapidly.
Stage two: valve of giving vent to anger is opened completely, and pass into sweeping gas and purge, the first reaction source residual in reaction chamber is extracted out.
At TMA after good self-diffusion, TMA is fully used.Now, close pneumavalve V3, the valve V9 that will give vent to anger opens completely, and open pneumavalve V2, V4, V5, using such as nitrogen or rare gas element as sweeping gas, pass in reaction chamber, the TMA of remnants purged clean and extracted out (as diagram dextrad hollow arrow indication, lower same) by vacuum pump.
In the stage three: the valve opening of giving vent to anger reducing reaction chamber, passes into the second reaction source, form the process to reaction chamber inflation, reaction chamber pressure is raised gradually, to increase effective diffusion time of the second reaction source.
TMA is purged totally, pneumavalve V2, V4, V5 are closed, and the aperture of the valve V9 that gives vent to anger is reduced, such as, the aperture of valve of giving vent to anger can be reduced to less than 1/3 of maximum opening.Then, open pneumavalve V7, in reaction chamber, pass into ozone as the second reaction source.In the process, because the aperture of valve of giving vent to anger obviously reduces, make the output of gas be less than air input, thus form the process to reaction chamber inflation, and the pressure in reaction chamber is raised gradually; Like this, the diffusion time of ozone can be increased.Meanwhile, ozone is compared the state that existing pressure remains unchanged within the scope of certain numerical value, can be carried out self-diffusion better, thus improve the utilization ratio of ozone under being in the pressure state constantly raised.
According to different processing requirements, as an optional embodiment, the pressure in reaction chamber can be made in the process to be increased to 0.5-10Torr gradually, be preferably 1-5Torr.Can be regulated the pressure in reaction chamber by valve system, make it be in the scope of needs.By making the pressure in reaction chamber raise gradually, reduce the requirement to reaction chamber pressure Controlling System; Also because of the raising of ozone self-diffusion ability, ozone can be spread more fully in reaction chamber, the utilization ratio of ozone can be improved equally, and improve the homogeneity of prepared film.
As one preferred embodiment, when passing into ozone, the aperture of valve of giving vent to anger can be reduced to zero, even if show that air valve is closed completely, thus the pressure in reaction chamber can be increased the most rapidly.
Stage four: valve of giving vent to anger is opened completely, and pass into sweeping gas and purge, the second reaction source remained in reaction chamber is extracted out.
At ozone after good self-diffusion, ozone is fully used.Now, close pneumavalve V7, the valve V9 that will give vent to anger opens completely, and opens pneumavalve V2, V4, V5, using such as nitrogen or rare gas element as sweeping gas, passes in reaction chamber, purges clean and extracted out the ozone of remnants by vacuum pump.
Now complete an aluminum oxide film growth cycle, can so circulate until complete the whole atomic layer deposition process of certain film thickness.
In following another embodiment of the present invention, the invention allows for the implementation method that a kind of technique for atomic layer deposition prepares film.Be described for deposited aluminum oxide thin film equally.Refer to Fig. 2, Fig. 2 is the implementation method schema that a kind of technique for atomic layer deposition in two of the better embodiment of the present invention one prepares film; Meanwhile, incorporated by reference to consulting Fig. 3.As shown in Figure 2, technique for atomic layer deposition of the present invention prepares the implementation method of film, can comprise following six stages:
Stage one: the valve opening of giving vent to anger reducing reaction chamber, passes into the first reaction source.
Refer to Fig. 3.When ALD technique starts, first, pneumavalve V1, V8, pneumavalve V2, V4, V5 and pneumavalve V6, pneumavalve V7 are closed; And the aperture of the valve V9 that gives vent to anger is reduced, such as the aperture of valve of giving vent to anger can be reduced to less than 1/3 of maximum opening.Then, open pneumavalve V3, in reaction chamber, pass into TMA as the first reaction source.
In the stage two: stop the first reaction source to pass into, and pass into diluent gas, form the process to reaction chamber inflation, reaction chamber pressure is raised gradually, to increase effective diffusion time of the first reaction source.
Then, pneumavalve V3 is closed, stop TMA passing into; Open pneumavalve V1, V8 of being located at diluent gas pipeline simultaneously, using such as nitrogen or rare gas element as diluent gas, pass in reaction chamber, TMA is diluted, remaining TMA in reaction chamber is uniformly distributed and promotes that it carries out self-diffusion.In the process, because the aperture of valve of giving vent to anger obviously reduces, make the output of gas be less than air input, thus form the process to reaction chamber inflation, and the pressure in reaction chamber is raised gradually; Like this, the diffusion time of TMA can be increased.Meanwhile, TMA compares the state that existing pressure remains unchanged within the scope of certain numerical value, can carry out self-diffusion better, thus improve the utilization ratio of TMA under being in the pressure state constantly raised.
As an optional embodiment, the pressure in reaction chamber can be made in the process to be increased to 0.5-10Torr gradually, be preferably 1-5Torr.Can be regulated the pressure in reaction chamber by valve system, make its be in needs scope in.This not only increases the utilization ratio of TMA, reduce process costs, and also reduce the requirement to reaction chamber pressure Controlling System, reduce equipment cost; TMA also can be made to have the longer time can spread in reaction chamber, thus improve the homogeneity of prepared film.
As one preferred embodiment, when passing into TMA, the aperture of valve of giving vent to anger can be reduced to zero, even if show that air valve is closed completely, thus the pressure in reaction chamber can be increased the most rapidly.
Stage three: valve of giving vent to anger is opened completely, and pass into sweeping gas and purge, the first reaction source residual in reaction chamber is extracted out.
At TMA after good self-diffusion, TMA is fully used.Now, close pneumavalve V1, V8, the valve V9 that will give vent to anger opens completely, and open pneumavalve V2, V4, V5 of being located at sweeping gas pipeline, using such as nitrogen or rare gas element as sweeping gas, pass in reaction chamber, the TMA of remnants is purged clean and is extracted out by vacuum pump.
Stage four: the valve opening of giving vent to anger reducing reaction chamber, passes into the second reaction source.
Then, pneumavalve V2, V4, V5 are closed, and the aperture of the valve V9 that gives vent to anger is reduced, such as, the aperture of valve of giving vent to anger can be reduced to less than 1/3 of maximum opening.Then, open the pneumavalve V7 being located at ozonizer pipeline, in reaction chamber, pass into ozone as the second reaction source.
Stage five: stop the second reaction source to pass into, and pass into diluent gas, form the process to reaction chamber inflation, reaction chamber pressure is raised gradually, to increase effective diffusion time of the second reaction source.
Then, pneumavalve V7 is closed, stop ozone passing into; Then, open pneumavalve V1, V8, equally using nitrogen or rare gas element as diluent gas, pass in reaction chamber, ozone is diluted, remaining ozone in reaction chamber is uniformly distributed and promotes that it carries out self-diffusion.In the process, because the aperture of valve of giving vent to anger obviously reduces, make the output of gas be less than air input, thus form the process to reaction chamber inflation, and the pressure in reaction chamber is raised gradually; Like this, the diffusion time of ozone can be increased.Meanwhile, ozone is compared the state that existing pressure remains unchanged within the scope of certain numerical value, can be carried out self-diffusion better, thus improve the utilization ratio of ozone under being in the pressure state constantly raised.
As an optional embodiment, the pressure in reaction chamber can be made in the process to be increased to 0.5-10Torr gradually, be preferably 1-5Torr.Can be regulated the pressure in reaction chamber by valve system, make it be in the scope of needs.This not only increases the utilization ratio of ozone, reduce process costs, and also reduce the requirement to reaction chamber pressure Controlling System, reduce equipment cost; Ozone also can be made to have the longer time can spread in reaction chamber, thus improve the homogeneity of prepared film.
As one preferred embodiment, when passing into ozone, the aperture of valve of giving vent to anger can be reduced to zero, even if show that air valve is closed completely, thus the pressure in reaction chamber can be increased the most rapidly.
Stage six: valve of giving vent to anger is opened completely, and pass into sweeping gas and purge, the second reaction source remained in reaction chamber is extracted out.
At ozone after good self-diffusion, ozone is fully used.Now, close pneumavalve V1, V8, the valve V9 that will give vent to anger opens completely, and open pneumavalve V2, V4, V5 of being located at sweeping gas pipeline, equally using nitrogen or rare gas element as sweeping gas, pass in reaction chamber, the ozone of remnants is purged clean, and extracted out by vacuum pump.
By above-mentioned six stage process, complete a growth cycle of aluminum oxide film, and can so circulate until complete the whole atomic layer deposition process of certain film thickness.
As optional embodiment, above-mentioned diluent gas also can directly adopt reaction source carrier gas or sweeping gas.Further, can also using sweeping gas pipeline simultaneously as diluent gas, sweeping gas pass into pipeline, and the diluent gas pipeline shown in Fig. 3 is separately used as him.
As other optional embodiments, in above-mentioned six stage process exemplified, wherein also diluent gas can not be passed in stage one, two or stage four, five, but when reduce reaction chamber give vent to anger valve opening, the only single reaction source passing into correspondence, form the process to reaction chamber inflation, reaction chamber pressure is raised gradually, to increase effective diffusion time of reaction source.The i.e. corresponding mode that have employed stage one in the above-mentioned four-stage technique exemplified or stage three, thus define the process form of following two kinds of double teachers:
The first double teacher technique is:
In the stage one: the valve opening of giving vent to anger reducing reaction chamber, passes into the first reaction source, form the process to reaction chamber inflation, reaction chamber pressure is raised gradually, to increase effective diffusion time of the first reaction source.
Stage two: valve of giving vent to anger is opened completely, and pass into sweeping gas and purge, the first reaction source residual in reaction chamber is extracted out.
Stage three: the valve opening of giving vent to anger reducing reaction chamber, passes into the second reaction source.
Stage four: stop the second reaction source to pass into, and pass into diluent gas, form the process to reaction chamber inflation, reaction chamber pressure is raised gradually, to increase effective diffusion time of the second reaction source.
Stage five: valve of giving vent to anger is opened completely, and pass into sweeping gas and purge, the second reaction source remained in reaction chamber is extracted out.
The second double teacher technique is:
Stage one: the valve opening of giving vent to anger reducing reaction chamber, passes into the first reaction source.
In the stage two: stop the first reaction source to pass into, and pass into diluent gas, form the process to reaction chamber inflation, reaction chamber pressure is raised gradually, to increase effective diffusion time of the first reaction source.
Stage three: valve of giving vent to anger is opened completely, and pass into sweeping gas and purge, the first reaction source residual in reaction chamber is extracted out.
In the stage four: the valve opening of giving vent to anger reducing reaction chamber, passes into the second reaction source, form the process to reaction chamber inflation, reaction chamber pressure is raised gradually, to increase effective diffusion time of the second reaction source.
Stage five: valve of giving vent to anger is opened completely, and pass into sweeping gas and purge, the second reaction source remained in reaction chamber is extracted out.
Below to prepare aluminum oxide (Al
2o
3) passivation film is example, aforesaid method according to the present invention provides following embodiment.