Reactive gas control system for reactive magnetron sputtering and debugging method
Technical Field
The invention belongs to the technical field of semiconductor manufacturing, and particularly relates to a reactive gas control system and a debugging method for reactive magnetron sputtering.
Background
Reactive magnetron sputtering is an improved magnetron sputtering technique, which introduces reactive gases based on conventional magnetron sputtering. The components and properties of the film can be changed by adding the reaction gas in the sputtering process, so that the film can be accurately regulated.
The process of reactive magnetron sputtering is similar to that of traditional magnetron sputtering, but is different in the gas injection link. Inert gas (such as argon) is used in the traditional magnetron sputtering to maintain a stable sputtering process, and gas containing reactive components is added in the reactive magnetron sputtering, so that chemical reaction occurs in the sputtering process.
By adding the reaction gas, the following functions can be achieved:
preparing an alloy film: by adding a gas containing an alloy component, the target and the reaction gas are reacted, and an alloy thin film is formed on the substrate.
Compound film preparation: by adding a gas containing a compound component, a target material and a reaction gas are chemically reacted, and a compound thin film is formed on a substrate.
Oxide film preparation: and (3) adding oxygen-containing gas to enable the metal element in the target material to react with oxygen to form the metal oxide film.
The reaction magnetron sputtering can realize the precise control of the components and the structure of the film, expands the application range of film preparation, and has important application value in the fields of material science, electronic devices, optical films and the like.
The reaction gas can react with sputtered metal atoms or ions on the surface of the target material to form a compound film. Common reactant gases include nitrogen, oxygen, argon, methane, and the like. Different reactant gases introduce different chemical elements, thereby affecting the chemical composition and structure of the film.
The concentration and flow rate of the reactant gases are important in controlling the composition of the film. Increasing the flow of the reactant gas increases the rate of the chemical reaction and increases the amount of compound in the deposited film. However, excessive reactant gas flow rates may result in excessive chemical reactions that produce undesirable film properties.
The effect of reactant gas distribution on film uniformity is very important. Uniform film deposition ensures that the film has a consistent thickness and composition across the substrate surface, thereby ensuring consistent film performance and function.
Uneven distribution of the reaction gas may cause the following problems:
1. Thickness non-uniformity: if the reactant gas distribution is uneven, the gas concentration in some regions is higher, while the gas concentration in other regions is lower, which results in a difference in film deposition rate in different regions, and eventually a film with uneven thickness is formed.
2. Component inhomogeneity: uneven distribution of the reactant gases can also lead to uneven film composition. In the partial region, the reactant gas concentration is higher, resulting in more chemical reactions occurring, forming different deposit compositions. This will result in differences in film composition in different regions.
3. Structural non-uniformity: the non-uniformity of the reactant gas distribution also affects the structure of the thin film. For example, in oxidation reactions, non-uniformity in oxygen concentration can lead to non-uniform formation of oxide phases, thereby affecting the crystal structure and performance of the thin film.
In order to ensure uniformity of the thin film, it is necessary to design a proper gas injection system, and by properly designing a gas supply system, it is ensured that the reaction gas is uniformly injected onto the target. There is no system architecture in the prior art that can meet the above needs.
Disclosure of Invention
In order to solve the problems, the invention discloses a reaction gas control system and a debugging method for reactive magnetron sputtering, which adopt pipelines which can control flow and are uniformly distributed to introduce gas into a magnetron sputtering cavity, so that the uniformity of a film can be improved.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
the debugging method of the reaction gas control system for the reaction magnetron sputtering comprises the following steps:
Step 1, setting the initial value of the gas flow of each valve in a multi-pipeline gas flow control system;
Step 2, introducing gas into the magnetron sputtering cavity through a multi-pipeline gas flow control system and a reaction gas flow divider; the multi-pipeline gas flow control system comprises a pipeline and n-level valves, wherein n is a natural number and is larger than or equal to 4; the reaction gas diverter comprises 2 n-1 gas pipelines which are led into the magnetron sputtering cavity, and the n-stage valve is used for diverting gas to the gas pipelines step by step;
Step 3, taking a plurality of measuring points on the surface of the film after the reaction is finished, and testing to obtain the resistance values of the measuring points;
Step 4, calculating variances of the resistance values of the measuring points obtained in the step 3, and dividing the variances by the average value of the resistance values of the measuring points to obtain a numerical value for representing the uniformity of the film;
Step 5, judging whether the value obtained in the step 4 is larger than a threshold value, and when the value is larger than the threshold value, indicating that the flow of part of the gas pipelines needs to be regulated, and entering the step 6; if the value is not greater than the threshold value, ending the debugging;
Step 6, obtaining measuring points deviating from a certain range of the average value of the resistance values of the measuring points, and performing compensation adjustment on the oxygen flow flowing through the measuring points to adjust the gas flow in the corresponding gas pipes at the measuring points; and repeatedly executing the steps 2-5.
Further, the measuring points are uniformly distributed on the surface of the film.
A reactive gas control system for reactive magnetron sputtering, comprising a multi-pipeline gas flow control system and a reactive gas splitter;
The multi-pipeline gas flow control system comprises a pipeline and n-level valves, wherein the n-level valve comprises a1 st-level valve, two 2 nd-level valves and four 3 rd-level valves … …,2 n-1 nth-level valves, and the 1 st-level valve is used for introducing gas into the multi-pipeline gas flow control system; from the 2 nd-stage valve, each two valves in the current-stage valve are respectively connected with a previous-stage valve through pipelines and are used for shunting the gas introduced from the previous-stage valve;
The reaction gas flow divider comprises 2 n-1 gas pipelines which are respectively connected with 2 n-1 nth-stage valves, and the gas pipelines are led into the magnetron sputtering cavity.
Further, the air outlets of the 2 n-1 air pipelines are uniformly distributed.
Further, the reaction gas flow divider further comprises a fixing ring, wherein the fixing ring is arranged in the magnetron sputtering cavity, and 2 n-1 gas pipelines are arranged on the fixing ring.
Further, solenoid valves are respectively arranged in front of the 1-stage valve and behind the n-stage valve.
Further, the n-stage valve adopts a manual valve or a mass flowmeter.
Further, when the n-stage valve adopts mass flow meter, the mass flow meter is controlled by the PLC.
The beneficial effects of the invention are as follows:
The reaction gas control system for the reaction magnetron sputtering adopts the multi-stage valves, the gas is fed into the cavity through the uniformly distributed multi-path gas flow divider, and the flow rate of the gas fed out by each valve is independently controlled by combining the measurement and calculation of the multipoint resistance value of the film after the reaction in the debugging method, so that the uniformity of the components of the film can be effectively improved and ensured. By adopting the system and the method provided by the invention, the gas can be directly and dispersedly introduced into the magnetron sputtering cavity from the reaction gas control system, the cavity opening operation is not needed, the operation steps are reduced, and the debugging time of the process is shortened.
Drawings
Fig. 1 is a schematic diagram of a multi-pipeline gas flow control system in a reactive gas control system for reactive magnetron sputtering.
FIG. 2 is a schematic diagram of a magnetron sputtering chamber.
Fig. 3 is a top view of a reactant gas splitter in a reactant gas control system for reactive magnetron sputtering.
Fig. 4 is a cross-sectional view of a reactant gas splitter in a reactant gas control system for reactive magnetron sputtering.
FIG. 5 is a schematic illustration of the measurement points of the surface of the film.
Reference numerals illustrate:
1: a1 st stage valve; 2-3: a2 nd stage valve; 4-7: a 3 rd stage valve; 8-15: a 4 th stage valve; 101: a wafer stage; 102: a target material; 103: a magnet; 104: a reactant gas splitter; 105: a fixing ring; 106: a gas line; 107: a Vcr joint; 108: and (3) a wafer.
Detailed Description
The technical scheme provided by the present invention will be described in detail with reference to the following specific examples, and it should be understood that the following specific examples are only for illustrating the present invention and are not intended to limit the scope of the present invention.
The invention designs a reaction gas control system for reaction magnetron sputtering, which comprises a multi-pipeline gas flow control system and a reaction gas diverter.
The overall structure of the multi-pipeline gas flow control system is shown in fig. 1, and the multi-pipeline gas flow control system comprises pipelines and 4-stage valves. Wherein the stage 1 valve comprises: a valve 1. The gas flow control range is 0-500sccm. The stage 2 valve includes: valve 2, valve 3. The gas flow control range of each level 2 valve is 0-250sccm. The stage 3 valve includes: valve 4, valve 5, valve 6, valve 7. The gas flow control range of each grade 3 valve is 0-100sccm. The stage 4 valve includes: valve 8, valve 9, valve 10, valve 11, valve 12, valve 13, valve 14, valve 15. The gas flow control range of each level 4 valve is 0-50sccm.
The valve 1 is connected with the valve 2 and the valve 3 respectively through pipelines, so as to control the gas flow through the valve 2 and the valve 3. The valve 2 is respectively connected with the valve 4 and the valve 5 through pipelines so as to control the flow of gas flowing through the valve 4 and the valve 5; the valve 3 is connected with the valve 6 and the valve 7 through pipelines respectively, so as to control the gas flow through the valve 6 and the valve 7. Likewise, the valve 4 is connected with the valve 8 and the valve 9 through pipelines respectively, so as to control the gas flow through the valve 8 and the valve 9; the valve 5 is respectively connected with the valve 10 and the valve 11 through pipelines so as to control the flow of gas flowing through the valve 10 and the valve 11; the valve 6 is respectively connected with the valve 12 and the valve 13 through pipelines so as to control the gas flow through the valve 12 and the valve 13; valve 7 is connected to valves 14, 15 via lines, respectively, to control the flow of gas through valves 14, 15. All the valves can be manual valves regulated by visual scales or mass flow meters with PLC control systems regulated by system set values.
The front of the level 1 valve (the front of the gas inflow direction and the rear of the gas outflow direction) and the rear of the level 4 valve are respectively connected with electromagnetic valves, and the electromagnetic valves can control the overall gas on-off of the multi-pipeline gas flow control system after being started. According to different application scenes, the electromagnetic valve can be connected to the front of the 1-stage valve or arranged behind the 4-stage valve independently, so that the control requirement is met.
The gas is introduced from the valve 1, so that the valve 1 is controlled to control the total amount of the reaction gas introduced into the magnetron sputtering cavity. The total amount of intake air is fixed. When the total amount of air intake is fixed, single flow control of 2-way 2-level gas pipelines (pipelines where 2-level valves are located), 4-way 3-level gas pipelines (pipelines where 3-level valves are located) and 8-way 4-level gas pipelines (pipelines where 3-level valves are located) can be respectively realized by adjusting the flow of each valve.
The multi-pipeline gas flow control system is arranged outside the magnetron sputtering cavity, and the reaction gas flow divider is arranged in the magnetron sputtering cavity. The magnetron sputtering cavity structure is shown in fig. 2, a wafer carrier 101, a target 102 and a magnet 103 are arranged in the cavity. The reaction gas splitter 104 is installed inside the magnetron sputtering chamber, and its top view structure is shown in fig. 3, and includes an annular fixing ring 105 adapted to the shape of the chamber, and eight uniformly distributed gas pipes 106 connected to the annular fixing ring. One end of each of the eight gas pipelines is fixed on the annular fixed ring, and the other end of each of the eight gas pipelines extends into the magnetron sputtering cavity. The interface of each gas pipeline fixed on the annular fixing ring is respectively connected with a 4 th-stage valve in the multi-pipeline gas flow control system through pipelines. The joint of the root parts of the eight air pipes fixed on the annular fixing ring can be connected with the 4 th-stage valve through an air pipeline after being provided with a 1/4 inch Vcr joint 107 in a sealing way. Eight gas pipelines can be connected in disorder, but are connected in sequence after fixing the starting point based on equipment debugging convenience. A cross-sectional view of the reactant gas splitter 104 is shown in fig. 4. The size of the gas pipeline is designed according to the sizes of the cavity and the wafer, and the gas distribution in the cavity is uniform by combining the debugging method.
The reaction gas flows through the multi-pipeline gas flow control system, then enters the reaction gas flow divider and finally enters the cavity. After active diffusion, uniform distribution is formed in the cavity.
In order to make the components of the magnetron sputtering oxide film uniform and in an ideal range, the reactive gas flow rate of different inlets in different directions needs to be compensated and adjusted in the cavity debugging stage, namely, different flow rates are selected at different positions in the 4-stage valve so as to control the components of the oxide film.
It should be noted that the 4-stage valve is only an example, and those skilled in the art can adjust the number of stages of the valve as required, preferably greater than or equal to 4 stages. For example, a 5-stage valve can be adopted, namely, after 8 4-stage gas pipelines, the pipeline is divided into 16 pipelines, and each pipeline is provided with one valve, and 16 valves are connected in total, so that the 5-stage valve is formed. Increasing the number of stages increases the number of gas lines that ultimately flow into the chamber, thereby increasing control accuracy, but with the consequent increase in cost. Those of ordinary skill in the art will select the appropriate number of stages of piping and valves as desired.
The specific debugging method of the reaction gas control system for the reaction magnetron sputtering comprises the following steps:
Step 1, setting the initial value of the gas flow of each valve in a multi-pipeline gas flow control system; table 1 below shows the initial flow rates of the valves in a specific example where the target material was Ti and the reactant gas introduced was O 2. It should be noted that the initial flow is uniformly distributed in this example, but this should not be taken as a limitation of the present invention, and one of ordinary skill in the art can adjust the initial flow value of each valve according to the need.
| Target material |
Ti |
| Valve number/mass flowmeter number |
Reactant gas flow/O 2 |
| 1 |
50sccm |
| 2 |
25sccm |
| 3 |
25sccm |
| 4 |
10sccm |
| 5 |
10sccm |
| 6 |
10sccm |
| 7 |
10sccm |
| 8 |
5sccm |
| 9 |
5sccm |
| 10 |
5sccm |
| 11 |
5sccm |
| 12 |
5sccm |
| 13 |
5sccm |
| 14 |
5sccm |
| 15 |
5sccm |
TABLE 1
As can be seen from the above table, the sum of the gas flows of the 2 nd stage is larger than the sum of the gas flows of the 3 rd stage, so that the pressure of the front stage is ensured to be larger than the pressure of the rear stage, and the backflow is avoided.
And 2, introducing gas into the magnetron sputtering cavity through a multi-pipeline gas flow control system and a reaction gas flow divider.
And step 3, taking a plurality of measuring points on the surface of the film after the reaction is finished, and testing the resistance values of the measuring points. As shown in fig. 5, in this example, 9 points (the number of the points is adjusted according to the need) are taken on the surface of the TiO 2 film obtained on the surface of the wafer 108 in a more dispersed manner, and the measured resistance values of the points at each point are shown in table 2:
| Point location |
Resistance KΩ |
| 1 |
150 |
| 2 |
142 |
| 3 |
148 |
| 4 |
149 |
| 5 |
144 |
| 6 |
155 |
| 7 |
153 |
| 8 |
171 |
| 9 |
165 |
TABLE 2
The number and the positions of the measurement points in fig. 5 are only taken as examples, and the number and the specific positions of the measurement points can be adjusted according to the needs during actual debugging, so that the measurement points are preferably uniformly distributed.
Step 4, calculating the variance of the resistance values of the measuring points obtained in the step 3, and dividing the variance by the average value of the resistance values of the measuring points; the uniformity of the TiO 2 film was 6.23%. The lower the number, the better the film uniformity.
And 5, judging whether the result obtained in the step 4 is greater than a threshold value, if so, indicating that the flow of part of the gas pipeline needs to be regulated, in the example, presetting the threshold value to be 3% (which can be regulated according to the requirement), and obviously, if the uniformity of the TiO 2 film is 6.23% greater than the threshold value, regulating the flow, and entering the step 6. If the flow rate of each gas pipeline is not greater than the threshold value, the flow rate of each gas pipeline is moderate, and the debugging is finished.
And 6, obtaining measuring points which deviate from the average value of the resistance values of all measuring points by a certain range, wherein the average value of the resistance is 153KΩ in the example, the resistance of the point ⑧、⑨ is larger and is 171KΩ and 165KΩ respectively, and the resistance exceeds the average value by more than 10KΩ, which means that the proportion of the film oxygen element at the corresponding position of the point ⑧、⑨ is larger, and the oxygen flow flowing through the position needs to be compensated and regulated, namely the oxygen flow in the corresponding gas pipeline at the position is reduced. In this example, since the number of the points with the resistance higher than the average value is greater than the number of the points with the resistance lower than the average value, the high-resistance points with larger deviation are selected as the adjustment points, and the oxygen flow at the adjustment points is reduced. If the number of the points with the resistance lower than the average value is more than that of the points with the resistance higher than the average value, the low-resistance point with larger deviation is selected as the adjusting point, and the oxygen flow in the corresponding gas pipeline at the position close to the adjusting point is increased. Through the adjusting mode, the number of pipelines needing to be adjusted in flow can be reduced, and operation steps and cost are saved. The corresponding gas pipeline at the adjusting point position is obtained by the following steps: and respectively calculating the distance between the outlet of each gas pipeline and the point ⑧、⑨, wherein if the distance is smaller than the adjustment threshold range, the gas pipeline with flow needing to be adjusted is obtained. The valve numbers of stage 4 connected to each gas line are shown in fig. 5, wherein the gas line outlets corresponding to valves 8, 9, 10, 15 are closer to point ⑧、⑨, and their flow rates are adjusted as shown in table 3 below:
| Target material |
Ti |
| Valve number/mass flowmeter number |
Reactant gas flow rate/O2 |
| 1 |
50sccm |
| 2 |
25sccm |
| 3 |
25sccm |
| 4 |
10sccm |
| 5 |
10sccm |
| 6 |
10sccm |
| 7 |
10sccm |
| 8 |
4.5sccm |
| 9 |
4.5sccm |
| 10 |
5.2sccm |
| 11 |
5sccm |
| 12 |
5sccm |
| 13 |
5sccm |
| 14 |
5sccm |
| 15 |
5.2sccm |
TABLE 3 Table 3
Step 2 to step 5 are performed again, and the 9 points in fig. 5 are still measured, and the resistance is shown in the following table 4:
| Point location |
Resistance KΩ |
| 1 |
147 |
| 2 |
144 |
| 3 |
149 |
| 4 |
148 |
| 5 |
145 |
| 6 |
154 |
| 7 |
153 |
| 8 |
153 |
| 9 |
154 |
TABLE 4 Table 4
The uniformity of the TiO 2 film obtained by the calculation in the step 4 is obviously improved, the uniformity is reduced from 6.23% to 2.63%, the uniformity is lower than a threshold value, and the debugging is finished.
It should be noted that the foregoing merely illustrates the technical idea of the present invention and is not intended to limit the scope of the present invention, and that a person skilled in the art may make several improvements and modifications without departing from the principles of the present invention, which fall within the scope of the claims of the present invention.