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CN105154848A - Method for preparing nitrogen oxygen silicon thin film - Google Patents

Method for preparing nitrogen oxygen silicon thin film Download PDF

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CN105154848A
CN105154848A CN201510483284.9A CN201510483284A CN105154848A CN 105154848 A CN105154848 A CN 105154848A CN 201510483284 A CN201510483284 A CN 201510483284A CN 105154848 A CN105154848 A CN 105154848A
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thin film
silicon oxynitride
radio frequency
deposition
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曹晓杰
刘忆军
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Piotech Inc
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Piotech Shenyang Co Ltd
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Abstract

氮氧硅薄膜的制备方法,主要解决现有技术使用热氧化和化学法进行气相沉积,存在沉积温度高及薄膜的各项指标不容易控制的问题。实现步骤:1、载物台控温:下电极通过热偶精确控制温度;2、装样:基板通过自动传片系统传入反应腔室;3、通气:从反应腔室内的上电极,即喷淋头,通入气体;4、沉积:由射频系统提供射频,通过等离子体技术沉积薄膜;5、后处理:停止通入主反应源硅烷,利用射频对薄膜表面进行后处理;6、抽真空:工艺停止。反应气体混合后通过喷淋头进入反应腔,反应腔引入射频功率进行沉积,可以得到高致密的薄膜。本发明能够实现薄膜的不同温度的沉积,通过反应参数的改变可得到不同性能、不同膜厚、不同折射率及不同消光系数的氮氧硅薄膜。可广泛地应用于半导体薄膜制造及应用技术领域。

The preparation method of the silicon oxynitride thin film mainly solves the problems of high deposition temperature and difficult control of various indexes of the thin film by thermal oxidation and chemical method for vapor deposition in the prior art. Implementation steps: 1. Temperature control of the stage: the lower electrode precisely controls the temperature through a thermocouple; 2. Sample loading: the substrate is transferred into the reaction chamber through the automatic transfer system; 3. Ventilation: from the upper electrode in the reaction chamber, namely Spray head, feed gas; 4. Deposition: The radio frequency system provides radio frequency, and deposit the film through plasma technology; 5. Post-processing: Stop feeding the main reaction source silane, and use radio frequency to post-treat the film surface; 6. Pumping Vacuum: process stopped. After the reaction gas is mixed, it enters the reaction chamber through the shower head, and the reaction chamber introduces radio frequency power for deposition, and a highly dense film can be obtained. The invention can realize the deposition of thin films at different temperatures, and silicon nitride oxide thin films with different properties, different film thicknesses, different refractive indices and different extinction coefficients can be obtained by changing the reaction parameters. It can be widely used in the field of semiconductor thin film manufacturing and application technology.

Description

氮氧硅薄膜的制备方法Preparation method of silicon oxynitride thin film

技术领域technical field

本发明涉及一种氮氧硅薄膜的制备方法,确切地说是一种使用等离子体化学气相沉积设备沉积氮氧硅薄膜的方法,属于半导体薄膜制造及应用技术领域。The invention relates to a method for preparing a silicon oxynitride film, specifically a method for depositing a silicon oxynitride film by using plasma chemical vapor deposition equipment, and belongs to the technical field of semiconductor film manufacture and application.

背景技术Background technique

在半导体集成电路中,绝缘介质薄膜被用于金属层间介质层、钝化层或减反射层,在半导体制备工艺中起着十分重要的作用。氮氧硅薄膜是一种新型的薄膜材料,具有很好的光学性能,多应用于半导体集成电路中的减反射层。传统的沉积氮氧硅薄膜的方法,使用热氧化和化学气相沉积,沉积温度高,薄膜的各项指标不容易控制。In semiconductor integrated circuits, insulating dielectric films are used as inter-metal dielectric layers, passivation layers or anti-reflection layers, and play a very important role in the semiconductor manufacturing process. Silicon oxynitride film is a new type of film material with good optical properties, and it is mostly used in the anti-reflection layer of semiconductor integrated circuits. The traditional method of depositing silicon oxynitride film uses thermal oxidation and chemical vapor deposition, the deposition temperature is high, and the various indicators of the film are not easy to control.

目前,随着半导体技术的不断发展,在集成电路中对薄膜的性能要求越来越高,等离子体化学气相沉积设备是一种沉积绝缘材料的一种新技术,使用该技术沉积氮氧硅薄膜温度较低,制备方法相对比较简单。通过射频和工艺参数的调整,可以得到不同的薄膜性能。At present, with the continuous development of semiconductor technology, the performance requirements of thin films in integrated circuits are getting higher and higher. Plasma chemical vapor deposition equipment is a new technology for depositing insulating materials. Using this technology to deposit silicon oxynitride thin films The temperature is low, and the preparation method is relatively simple. Through the adjustment of radio frequency and process parameters, different film properties can be obtained.

发明内容Contents of the invention

本发明以解决上述问题为目的,主要解决现有技术使用热氧化和化学法进行气相沉积,存在沉积温度高及薄膜的各项指标不容易控制的问题。The purpose of the present invention is to solve the above problems, and mainly solve the problems of high deposition temperature and difficult control of various indexes of the film in the prior art using thermal oxidation and chemical methods for vapor deposition.

为实现上述目的,本发明提供了一种氮氧硅薄膜的制备方法,该方法采用等离子体化学气相沉积设备来沉积氮氧硅薄膜,通过反应参数的改变可得到不同性能的薄膜。To achieve the above object, the present invention provides a method for preparing a silicon oxynitride film, which uses plasma chemical vapor deposition equipment to deposit a silicon oxynitride film, and films with different properties can be obtained by changing the reaction parameters.

本发明是通过下述具体步骤实现的:The present invention is achieved through the following specific steps:

1)载物台控温:下电极通过热偶精确控制温度;1) Stage temperature control: the lower electrode precisely controls the temperature through a thermocouple;

2)装样:基板通过自动传片系统传入反应腔室;2) Sample loading: the substrate is introduced into the reaction chamber through the automatic transfer system;

3)通气:从反应腔室内的上电极,即喷淋头,通入气体硅烷、笑气、氦气和氮气;3) Ventilation: from the upper electrode in the reaction chamber, that is, the shower head, gas silane, laughing gas, helium and nitrogen are introduced;

4)沉积:由射频系统提供射频,通过等离子体技术沉积薄膜;4) Deposition: The radio frequency is provided by the radio frequency system, and the thin film is deposited by plasma technology;

5)后处理:停止通入主反应源硅烷,利用射频对薄膜表面进行后处理;5) post-treatment: stop feeding the main reaction source silane, and use radio frequency to carry out post-treatment on the film surface;

6)抽真空:工艺停止,反应腔室抽至真空。6) Vacuuming: the process is stopped, and the reaction chamber is evacuated to vacuum.

进一步地,所述氮氧硅薄膜制备方法,其特征在于:该氮氧硅薄膜的沉积温度可由150℃-450℃。Further, the method for preparing the silicon oxynitride film is characterized in that: the deposition temperature of the silicon oxynitride film can be from 150°C to 450°C.

进一步地,所述氮氧硅薄膜制备方法,其特征在于:反应气体为硅烷、笑气、氦气和氮气。Further, the preparation method of silicon oxynitride thin film is characterized in that: the reaction gas is silane, laughing gas, helium and nitrogen.

进一步地,所述氮氧硅薄膜制备方法,其特征在于:反应气体中硅烷与笑气的比为1:1到1:5,硅烷的流量为100sccm-500sccm;笑气的流量为300sccm-1500sccm;氦气流量为1000sccm—9000sccm,氮气流量为300sccm-7000sccm。Further, the preparation method of silicon oxynitride thin film is characterized in that: the ratio of silane to laughing gas in the reaction gas is 1:1 to 1:5, the flow rate of silane is 100 sccm-500 sccm; the flow rate of laughing gas is 300 sccm-1500 sccm ; The flow rate of helium is 1000sccm-9000sccm, and the flow rate of nitrogen gas is 300sccm-7000sccm.

进一步地,所述氮氧硅薄膜制备方法,其特征在于:反应压力1-7Torr。Further, the method for preparing the silicon oxynitride thin film is characterized in that the reaction pressure is 1-7 Torr.

进一步地,所述氮氧硅薄膜制备方法,其特征在于:通过载物台的上下运动,来控制上下电极之间的距离。Further, the method for preparing the silicon oxynitride thin film is characterized in that the distance between the upper and lower electrodes is controlled by moving the stage up and down.

进一步地,所述氮氧硅薄膜制备方法,其特征在于:反应过程中,射频功率可由100w-1000w。Further, the preparation method of silicon oxynitride thin film is characterized in that: during the reaction process, the radio frequency power can be from 100w to 1000w.

进一步地,所述氮氧硅薄膜制备方法,其特征在于:在沉积结束后,通过射频对薄膜表面进行后处理,此时停止通入主反应源硅烷。Further, the method for preparing the silicon oxynitride thin film is characterized in that after the deposition is completed, the surface of the thin film is post-treated by radio frequency, and at this time, the main reaction source silane is stopped.

进一步地,所述氮氧硅薄膜制备方法,其特征在于:薄膜的沉积速率可达到1000-4000A/min。Further, the method for preparing the silicon oxynitride thin film is characterized in that the deposition rate of the thin film can reach 1000-4000A/min.

进一步地,所述氮氧硅薄膜制备方法,其特征在于:反应基板可以是硅片或玻璃。Furthermore, the method for preparing the silicon oxynitride thin film is characterized in that: the reaction substrate may be a silicon wafer or glass.

本发明的有益效果及特点在于:Beneficial effects and characteristics of the present invention are:

本发明所采用的使用等离子体增强化学气相沉积的方法来制备氮氧硅薄膜,其制备方法能够实现薄膜的不同温度的沉积,通过改变不同气体的流量比,可以得到不同膜厚,不同折射率,不同消光系数的氮氧硅薄膜。可广泛地应用于半导体薄膜制造及应用技术领域。The method of plasma enhanced chemical vapor deposition used in the present invention is used to prepare silicon oxynitride thin films. The preparation method can realize the deposition of thin films at different temperatures. By changing the flow ratio of different gases, different film thicknesses and different refractive indices can be obtained. , SiON films with different extinction coefficients. It can be widely used in the field of semiconductor thin film manufacturing and application technology.

附图说明Description of drawings

图1是本发明所使用设备的反应腔示意图Fig. 1 is the reaction chamber schematic diagram of equipment used in the present invention

具体实施方式Detailed ways

下面结合具体实施例对本发明的沉积方法做进一步详细说明。根据下面说明,本发明的优点和特征将更清楚。本发明使用沈阳拓荆科技有限公司生产的等离子体增强化学气相沉积设备。设备的反应腔系统如图1所示。The deposition method of the present invention will be further described in detail below in conjunction with specific examples. The advantages and features of the present invention will become clearer from the following description. The present invention uses plasma-enhanced chemical vapor deposition equipment produced by Shenyang Tuojing Technology Co., Ltd. The reaction chamber system of the equipment is shown in Figure 1.

实施例1:Example 1:

本发明第一实例制备氮氧硅薄膜的方法,具体步骤如下:The first example of the present invention prepares the method for silicon oxynitride thin film, concrete steps are as follows:

1)沉积腔室载物台如图1中反应腔载物台2,即加热盘的温度为400℃,1) The stage of the deposition chamber is as shown in the reaction chamber stage 2 in Figure 1, that is, the temperature of the heating plate is 400°C,

其控制方式为通过热电偶实时监测和控制温度Its control method is to monitor and control the temperature in real time through thermocouples

2)将晶圆3放入反应腔载物台2上,通过上电极喷淋头1向反应腔室通入气体硅烷、笑气、氦气及氮气,气体流量分别为硅烷为300sccm;笑气为1100sccm;氦气为5000sccm;氮气为900sccm。2) Put the wafer 3 on the stage 2 of the reaction chamber, pass the gas silane, laughing gas, helium and nitrogen into the reaction chamber through the upper electrode shower head 1, and the gas flow rate is 300 sccm for silane; 1100sccm; 5000sccm for helium; 900sccm for nitrogen.

3)在腔室通气的同时,设置反应腔室压力为3.5torr,此压力即为沉积过程中的反应压力;3) While the chamber is being ventilated, set the reaction chamber pressure to 3.5 torr, which is the reaction pressure during the deposition process;

4)在通气步骤基础上,由射频系统提供射频开始薄膜沉积过程,4) On the basis of the ventilation step, the radio frequency is provided by the radio frequency system to start the film deposition process,

使用不同的射频反应功率进行氮氧硅薄膜的沉积,结果如下表:Using different RF reaction powers to deposit silicon oxynitride films, the results are shown in the following table:

表1Table 1

实施例1中显示通过改变反应的射频功率,薄膜的沉积速率可以随之增加。Example 1 shows that by changing the RF power of the reaction, the deposition rate of the film can be increased accordingly.

实施方式2:Implementation mode 2:

本发明第二实例制备氮氧硅薄膜的方法,具体步骤如下:The second example of the present invention prepares the method for silicon oxynitride thin film, concrete steps are as follows:

1)沉积腔室载物台如图1中反应腔载物台2,即加热盘温度为400℃,其1) The stage of the deposition chamber is as shown in the reaction chamber stage 2 in Figure 1, that is, the temperature of the heating plate is 400°C, and

控制方式为通过热电偶实时监测和控制温度The control method is to monitor and control the temperature in real time through thermocouples

2)将晶圆3放入反应腔载物台2上,通过上电极喷淋头1向反应腔室通入气体硅烷、笑气、氦气及氮气,改变硅烷和笑气流量比,270/900,285/1000,300/1100,315/1200和330/1300sccm。2) Put the wafer 3 on the stage 2 of the reaction chamber, pass the gas silane, nitrous oxide, helium and nitrogen into the reaction chamber through the upper electrode shower head 1, and change the flow ratio of silane and nitrous oxide, 270/ 900, 285/1000, 300/1100, 315/1200 and 330/1300 sccm.

3)在腔室通气的同时,设置反应腔室压力为3.5torr,此压力即为沉积过程中的反应压力;3) While the chamber is being ventilated, set the reaction chamber pressure to 3.5 torr, which is the reaction pressure during the deposition process;

4)在通气步骤基础上,由射频系统提供射频,射频功率为300W开始薄膜沉积过程。4) On the basis of the aeration step, the radio frequency is provided by the radio frequency system, and the radio frequency power is 300W to start the film deposition process.

在此实施例中,结果如下表:In this example, the results are as follows:

表2Table 2

实施例2中显示通过改变反应气体硅烷和笑气的流量比,同样可以改变沉积速率,同时可以改变薄膜的光学常数,实现薄膜在半导体集成电路中的不同应用。Example 2 shows that by changing the flow ratio of the reaction gas silane and laughing gas, the deposition rate can also be changed, and at the same time the optical constants of the film can be changed to realize different applications of the film in semiconductor integrated circuits.

Claims (9)

1.一种氮氧硅薄膜的制备方法,其特征在于:该方法是通过下述具体步骤实现的:1. a preparation method of silicon oxynitride film, is characterized in that: the method is realized by following specific steps: (1)载物台控温:下电极通过热偶精确控制温度;(1) Stage temperature control: the lower electrode precisely controls the temperature through a thermocouple; (2)装样:反应基板通过自动传片系统传入反应腔室;(2) Sample loading: the reaction substrate is introduced into the reaction chamber through the automatic transfer system; (3)通气:从反应腔室内的上电极,即喷淋头,通入气体硅烷、笑气、氦气和氮气;(3) Ventilation: from the upper electrode in the reaction chamber, that is, the shower head, gas silane, laughing gas, helium and nitrogen are introduced; (4)沉积:由射频系统提供射频,通过等离子体技术沉积薄膜;(4) Deposition: The radio frequency is provided by the radio frequency system, and the thin film is deposited by plasma technology; (5)后处理:停止通入主反应源硅烷,利用射频对薄膜表面进行后处理;(5) post-treatment: stop feeding the main reaction source silane, and use radio frequency to carry out post-treatment on the film surface; (6)抽真空:工艺停止,反应腔室抽至真空。(6) Vacuuming: the process is stopped, and the reaction chamber is evacuated to vacuum. 2.如权利要求1所述的氮氧硅薄膜的制备方法,其特征在于:所述氮氧硅薄膜的沉积温度由150℃-450℃;反应压力1-7Torr。2 . The method for preparing a silicon oxynitride film according to claim 1 , wherein the deposition temperature of the silicon oxynitride film is from 150° C. to 450° C.; the reaction pressure is 1-7 Torr. 3.如权利要求1所述的氮氧硅薄膜的制备方法,其特征在于:所述反应气体为硅烷、笑气、氦气和氮气。3. The method for preparing a silicon oxynitride thin film according to claim 1, characterized in that: the reaction gas is silane, laughing gas, helium and nitrogen. 4.如权利要求1所述的氮氧硅薄膜的制备方法,其特征在于:所述反应气体中硅烷与笑气的比为1:1至1:5,硅烷的流量为100sccm-500sccm;笑气的流量为300sccm-1500sccm;氦气流量为1000sccm—9000sccm;氮气流量为300sccm-7000sccm,反应气体混合后通过喷淋头进入反应腔,反应腔引入射频功率进行沉积,可以得到高致密的薄膜。4. the preparation method of silicon oxynitride film as claimed in claim 1 is characterized in that: the ratio of silane and laughing gas in the reaction gas is 1:1 to 1:5, and the flow rate of silane is 100sccm-500sccm; The flow rate of gas is 300sccm-1500sccm; the flow rate of helium gas is 1000sccm-9000sccm; the flow rate of nitrogen gas is 300sccm-7000sccm. After the reaction gas is mixed, it enters the reaction chamber through the shower head, and the reaction chamber introduces radio frequency power for deposition, so that a highly dense film can be obtained. 5.如权利要求1所述的氮氧硅薄膜的制备方法,其特征在于:该方法是通过载物台的上下运动,来控制上下电极之间的距离。5 . The method for preparing a silicon oxynitride thin film according to claim 1 , wherein the method is to control the distance between the upper and lower electrodes by moving the stage up and down. 6 . 6.如权利要求1所述的氮氧硅薄膜的制备方法,其特征在于:反应过程中,射频功率由100w-1000w。6. The method for preparing silicon oxynitride film according to claim 1, characterized in that: during the reaction process, the radio frequency power ranges from 100w to 1000w. 7.如权利要求1所述的氮氧硅薄膜的制备方法,其特征在于:在沉积结束后,通过射频对薄膜表面进行后处理,此时停止通入主反应源硅烷。7. The method for preparing a silicon oxynitride thin film according to claim 1, characterized in that: after the deposition, the surface of the thin film is post-treated by radio frequency, and at this time, the main reaction source silane is stopped. 8.如权利要求1所述的氮氧硅薄膜的制备方法,其特征在于:薄膜的沉积速率为1000-4000A/min。8 . The method for preparing a silicon oxynitride thin film according to claim 1 , wherein the deposition rate of the thin film is 1000-4000 A/min. 9.如权利要求1所述的氮氧硅薄膜的制备方法,其特征在于:所述反应基板的材质为硅片或玻璃。9. The method for preparing a silicon oxynitride thin film according to claim 1, wherein the reaction substrate is made of silicon wafer or glass.
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CN110684966A (en) * 2019-10-16 2020-01-14 江苏鲁汶仪器有限公司 Method for growing compact film in PECVD mode
CN114622183A (en) * 2020-12-11 2022-06-14 湖南红太阳光电科技有限公司 Method for preparing silicon oxide film
CN114975113A (en) * 2022-04-25 2022-08-30 上海陛通半导体能源科技股份有限公司 Method for forming silicon oxide and silicon nitride composite film

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CN114975113B (en) * 2022-04-25 2022-12-13 上海陛通半导体能源科技股份有限公司 Method for forming silicon oxide and silicon nitride composite film

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