WO2022089288A1 - 氧化物薄膜的制备方法 - Google Patents

氧化物薄膜的制备方法 Download PDF

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WO2022089288A1
WO2022089288A1 PCT/CN2021/125198 CN2021125198W WO2022089288A1 WO 2022089288 A1 WO2022089288 A1 WO 2022089288A1 CN 2021125198 W CN2021125198 W CN 2021125198W WO 2022089288 A1 WO2022089288 A1 WO 2022089288A1
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target
equal
less
radio frequency
gas
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PCT/CN2021/125198
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English (en)
French (fr)
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罗建恒
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北京北方华创微电子装备有限公司
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Priority to EP21885015.4A priority Critical patent/EP4234756A1/en
Priority to US18/250,541 priority patent/US20230399734A1/en
Priority to KR1020237013507A priority patent/KR20230072489A/ko
Priority to JP2023524557A priority patent/JP7522931B2/ja
Publication of WO2022089288A1 publication Critical patent/WO2022089288A1/zh

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Definitions

  • the present invention relates to the field of semiconductor technology, and more particularly, to a method for preparing an oxide film.
  • etch stop layer is usually deposited on the interlayer dielectric layer and the metal lines. The etch stop layer is used to protect the material covered by the etch stop layer during the patterning process of the integrated circuit manufacturing process. is not etched during this period. This etch stop layer is usually not completely removed and ends up remaining in the fabricated semiconductor device.
  • Alumina is increasingly used as an etch stop layer due to its good process compatibility.
  • a commonly used method for preparing aluminum oxide films is chemical vapor deposition (Chemical Vapor Deposition, hereinafter referred to as CVD) method, but the films prepared by this CVD method have many impurities, low density and high process cost.
  • CVD chemical vapor deposition
  • PVD physical vapor deposition
  • the aluminum oxide film prepared by the PVD method has good film uniformity, less impurities and high density. It is one of the most commonly used methods in the metallization process of integrated circuits.
  • the purpose of the present invention is to propose a preparation method of an oxide film, which solves the problems of low deposition rate, particle defects, large surface roughness and low film density during the process.
  • the preparation method includes:
  • Step 1 Put the wafer to be deposited on the base of the reaction chamber
  • Step 2 Pour the first mixed gas of bombardment gas and oxidizing gas into the reaction chamber, apply DC power and radio frequency power to the target, and excite the first mixed gas to form plasma, so as to bombard the target at forming an oxide film on the wafer;
  • Step 3 Stop applying DC power and radio frequency power to the target material, pass a second mixed gas of bombardment gas, oxidizing gas and nitrogen into the reaction chamber, apply radio frequency power to the base, and excite the second mixed gas to form plasma to form a plasma. Bombarding the oxide film to form an oxynitride film;
  • Step 4 Continue to pass the second mixed gas into the reaction chamber, apply DC power and radio frequency power to the target, continue to apply radio frequency power to the base, and excite the second mixed gas to form plasma body to bombard the target material and the oxynitride film formed in the step 3, so as to form an oxynitride film on the oxynitride film formed in the step 3.
  • the DC power applied to the target is less than 10000W, and the radio frequency power applied to the target is less than 3000W, wherein the radio frequency power applied to the target is the same as that applied to the target.
  • the ratio of the DC power applied by the target is greater than or equal to 2 and less than or equal to 4.
  • the DC power applied to the target is greater than or equal to 100W and less than or equal to 200W, and the radio frequency power applied to the target is greater than or equal to 300W and less than or equal to 600W, wherein, the ratio of the radio frequency power applied to the target to the DC power applied to the target is 3.
  • the DC power applied to the target material is less than 10000W, and the radio frequency power applied to the target material is less than 3000W, wherein the radio frequency power applied to the target material is the same as that applied to the target material.
  • the ratio of the DC power applied by the target material is greater than or equal to 2 and less than or equal to 7.
  • the DC power applied to the target is greater than or equal to 3000W and less than or equal to 6000W, and the radio frequency power applied to the target is greater than or equal to 1000W and less than or equal to 2000W, wherein, the ratio of the radio frequency power applied to the target to the DC power applied to the target is greater than or equal to 3 and less than or equal to 6.
  • the sum of the flow rates of the oxidizing gas and the nitrogen gas is greater than the flow rate of the bombarding gas.
  • the radio frequency power applied to the base is less than 500W.
  • the process conditions in step 1 are: the vacuum degree of the reaction chamber is less than 5 ⁇ 10-6 Torr; the temperature of the susceptor is greater than or equal to 250°C and less than or equal to 350°C.
  • the flow rate of the bombardment gas is less than 500 sccm, and the flow rate of the oxidizing gas is less than 500 sccm, wherein the flow rate of the bombardment gas is greater than that of the oxidizing gas traffic.
  • the target material includes an aluminum, titanium, silicon, hafnium or tantalum target material, or a compound target material including aluminum, titanium, silicon, hafnium or tantalum.
  • step 2 DC power and radio frequency power are simultaneously applied to the target material, which can reduce the generation of particle defects in the oxide deposition process.
  • step 3 a second mixed gas of bombardment gas, oxidizing gas and nitrogen gas is introduced, and radio frequency power is applied to the susceptor, which can not only generate an oxynitride film in situ, but also perform certain etching on the surface of the oxide film. , so that the surface roughness of the oxide film can be reduced while reducing the surface defects of the oxide film.
  • step 4 the above-mentioned second mixed gas is continuously introduced, and at the same time, DC power and RF power are applied to the target material, and RF power is applied to the susceptor, so that high-density, low-roughness oxynitride can be deposited on the wafer surface. Therefore, the quality of the film can be improved, and the high-quality surface of the film can also inhibit the formation of a transition layer between the etching layer and the metal layer, thereby reducing the oxidation of the metal layer.
  • FIG. 1 shows a flow chart of steps of a method for preparing an oxide thin film according to an embodiment of the present invention.
  • FIG. 2 is a graph showing a comparison of the number of particle defects in oxide thin films prepared according to an embodiment of the present invention and the prior art.
  • FIG. 3 shows a comparison diagram of etching uniformity of oxide thin films prepared according to an embodiment of the present invention and the prior art.
  • FIG. 1 shows a flow chart of the steps of a method for preparing an oxide thin film according to an embodiment of the present invention. Please refer to FIG. 1, the preparation method of the oxide film includes:
  • Step 1 Put the wafer to be deposited on the base of the reaction chamber
  • Step 2 Pour the first mixed gas of bombardment gas and oxidizing gas into the reaction chamber, apply DC power and radio frequency power to the target material, excite the first mixed gas to form plasma, and bombard the target material to form oxidation on the wafer material film;
  • Step 3 stop applying the DC power and the radio frequency power to the target, pass the second mixed gas of bombardment gas, oxidizing gas and nitrogen into the reaction chamber, apply radio frequency power to the base, and excite the second mixed gas to form plasma , to form an oxynitride film by bombarding the oxide film;
  • Step 4 Continue to feed the second mixed gas into the reaction chamber, apply DC power and radio frequency power to the target, continue to apply radio frequency power to the base, and excite the second mixed gas to form plasma to bombard the target and the above steps
  • the oxynitride film formed in step 3 to form an oxynitride film on the oxynitride film formed in the above step 3.
  • the preparation of the film is carried out in a reaction chamber, which is provided with a susceptor for carrying the wafer on which the film is to be deposited, the susceptor having heating and/or cooling functions so as to be able to control the temperature of the wafer.
  • the reaction chamber is connected with a vacuum system, and the vacuum system can evacuate the reaction chamber, so that the reaction chamber can reach the required vacuum degree to meet the vacuum conditions required by the process.
  • Gases required for the process (such as bombardment gas, oxidizing gas, etc.) are introduced into the reaction chamber through an inlet line, and a flow meter can be set on the inlet line to control the flow of the gas.
  • the targets required for the process are sealed in the upper area of the reaction chamber (above the susceptor).
  • the above target can be pure metal or metal compound, or silicon or silicon dioxide (when silicon oxides need to be deposited).
  • the power supply will apply power to the target to make it negatively biased relative to the grounded reaction chamber.
  • the high voltage causes the bombardment gas and oxidizing gas to ionize and discharge to generate a positively charged plasma, which is positively charged.
  • the plasma is attracted by the target and bombards the target. When the energy of the plasma is high enough, atoms on the surface of the target escape and deposit on the wafer, enabling the deposition of thin films on the wafer surface.
  • a method for preparing an oxide film is described in detail by taking the deposition of a composite film of aluminum oxide and aluminum oxynitride on the surface of a wafer as an example.
  • step 1 is performed, according to the different films to be deposited, suitable process conditions are set for the reaction chamber, the wafers to be deposited films are placed on the base of the reaction chamber, and the base temperature is adjusted to the requirements of the process temperature.
  • the preparation method is used to deposit an aluminum oxide film.
  • the set process conditions are that the vacuum degree of the reaction chamber is less than 5 ⁇ 10 -6 Torr; the temperature of the base is greater than or equal to 250 °C, and less than or equal to 350 °C, preferably, such as 300 °C.
  • Step 2 the first mixed gas of bombardment gas and oxidizing gas is introduced into the reaction chamber, DC power and radio frequency power are applied to the target material, and the first mixed gas is excited to form plasma, so as to bombard the target material to form on the wafer oxide film.
  • the pulsed DC power has two stages of positive voltage and negative voltage in one cycle.
  • the power supply loads a negative voltage on the target, and the plasma will bombard the target to achieve sputtering of the target; in the positive voltage stage, the DC power supply loads a positive voltage on the target, and electrons will be introduced into the target at this time to neutralize the target. and the positive charge accumulated on the surface of the target.
  • the loading method of this pulsed DC power will lead to low deposition rate, uneven etching, particle defects caused by frequent abnormal arc discharge, large surface roughness of the film, low film density, and easy adsorption of water, oxygen, Problems such as the formation of surface defects by impurity gases such as carbon have caused great difficulties in subsequent process integration.
  • step 2 of this embodiment DC power and RF power are simultaneously applied to the target material.
  • This RF/DC co-sputtering power loading method can form a negative voltage on the target material, thereby promoting plasma Bombard the target to achieve sputtering of the target.
  • This RF/DC co-sputtering power loading method also reduces ion energy and avoids damage to the interlayer dielectric (ILD) film at the bottom of the wafer, allowing the formation of high-density aluminum oxide films (for example, as a contact layer)
  • ILD interlayer dielectric
  • it can also reduce the generation of particle defects during the deposition of metal oxides, and at the same time, in the process of depositing nitrogen oxide films, it can inhibit the adsorption of water, oxygen and carbon in the air on the surface of metal oxides to generate particle defects.
  • increasing the radio frequency power on the target can increase the collision ionization of oxygen in the plasma, change the distribution of oxygen atoms, and improve the uniformity of wet etching of oxide films.
  • step 3 stop applying DC power and radio frequency power to the target material, pass a second mixed gas of bombardment gas, oxidizing gas and nitrogen into the reaction chamber, apply radio frequency power to the base, and excite the second mixed gas to form plasma,
  • the oxynitride film is formed by bombarding the oxide film.
  • applying radio frequency power to the susceptor can form a negative bias voltage on the susceptor to attract plasma to bombard the surface of the film, so as to achieve the purpose of treating the surface of the oxide film formed in step 2.
  • This surface The treatment can form an oxynitride film in situ, that is, a thinner oxynitride film is formed on the surface of the oxide film to reduce surface defects of the oxide film; at the same time, the above surface treatment can also affect the surface of the formed oxide film. A certain amount of etching is performed to reduce the roughness of the film surface.
  • Carry out step 4 continue to pass the above-mentioned second mixed gas into the reaction chamber, apply DC power and radio frequency power to the target material, continue to apply radio frequency power to the base, and excite the second mixed gas to form plasma to bombard the target material and the above-mentioned
  • the oxynitride film formed in step 3 is to form an oxynitride film on the oxynitride film (or oxide film) formed in step 3 above.
  • DC power and RF power are applied to the target at the same time, and RF power is applied to the base, so that the film can be etched and deposited at the same time, and the deposition rate is greater than the etching rate, so that the film can be etched and deposited on the wafer surface.
  • the deposition forms a high-density, low-roughness film, which can improve the film quality, and the high-quality film surface can also inhibit the formation of a transition layer between the etched layer and the metal layer, which can reduce the oxidation of the metal layer.
  • the bombarding gas is, for example, argon
  • the oxidizing gas is, for example, oxygen
  • step 2 the process pressure of the reaction chamber is maintained at greater than or equal to 3 mTorr and less than or equal to 10 mTorr.
  • the flow rate of the bombarding gas is less than 500 sccm. In a preferred embodiment, the flow rate of the bombarding gas is greater than or equal to 50 sccm and less than or equal to 200 sccm; the flow rate of the oxidizing gas is less than 500 sccm, in a preferred embodiment , the flow rate of the oxidizing gas is greater than or equal to 20sccm and less than or equal to 100sccm. Wherein, the flow rate of the bombardment gas is greater than the flow rate of the oxidizing gas, that is, the ratio of the bombardment gas to the oxidizing gas is greater than 1.
  • the present embodiment reduces the proportion of oxidizing gas compared with the prior art, which can avoid excessive proportion of oxidizing gas High, the proportion of oxidizing gas is too high, which is not conducive to the control of particle defects and etching uniformity, and can also reduce the generation of particle defects during the deposition of metal oxides.
  • the adsorption of water, oxygen, and carbon on the surface of metal oxides produces particle defects.
  • the DC power applied to the target material is less than 10000W. In a preferred embodiment, the DC power is greater than or equal to 100W and less than or equal to 200W.
  • the radio frequency power applied to the target material is less than 3000W. In a preferred embodiment, the radio frequency power is greater than or equal to 300W and less than or equal to 600W.
  • the ratio of the radio frequency power applied to the target to the DC power applied to the target is greater than or equal to 2 and less than or equal to 4. In a preferred embodiment, the ratio is 3.
  • the ionization and collision of aluminum and oxygen atoms in high-density plasma can be increased when the aluminum oxide film is deposited, and the lateral migration of the film during growth on the substrate surface can be changed. Thereby, a low-damage, high-density thin film is formed, so as to avoid damage to the interlayer dielectric layer with low dielectric constant at the bottom layer, and change the dielectric constant of the material.
  • the bombarding gas is, for example, argon
  • the oxidizing gas is, for example, oxygen.
  • the nitrogen gas is used to bombard the surface of the formed oxide film to a certain extent after ionization.
  • step 3 the process pressure of the reaction chamber is maintained at greater than or equal to 3 mTorr and less than or equal to 10 mTorr.
  • the flow rate of the bombarding gas is less than 500 sccm.
  • the flow rate of the bombarding gas is greater than or equal to 50 sccm and less than or equal to 200 sccm; the flow rate of the oxidizing gas is less than 500 sccm, the preferred embodiment Among them, the flow rate of the oxidizing gas is greater than or equal to 20 sccm and less than or equal to 100 sccm.
  • the sum of the flow rates of the oxidizing gas and the nitrogen gas is greater than the flow rate of the bombarding gas, that is, the ratio of the sum of the flow rates of the oxidizing gas and the nitrogen gas to the flow rate of the bombarding gas is greater than 1. This arrangement helps to perform certain etching on the surface of the formed oxide film, so as to reduce the roughness of the film surface.
  • the radio frequency power applied to the base is less than 500W. In a preferred embodiment, the range of radio frequency power applied to the base is greater than or equal to 50W and less than or equal to 100W.
  • step 4 the process pressure of the reaction chamber is maintained at greater than or equal to 3 mTorr and less than or equal to 10 mTorr.
  • the flow rate of the bombarding gas is less than 500 sccm. In a preferred embodiment, the flow rate of the bombarding gas is greater than or equal to 50 sccm and less than or equal to 200 sccm; the flow rate of the oxidizing gas is less than 500 sccm, in a preferred embodiment , the flow rate of the oxidizing gas is greater than or equal to 20sccm and less than or equal to 100sccm. Wherein, the flow rate of the bombardment gas is greater than the flow rate of the oxidizing gas, that is, the ratio of the bombardment gas to the oxidizing gas is greater than 1.
  • the DC power applied to the target is less than 10000W.
  • the DC power is greater than or equal to 3000W and less than or equal to 6000W;
  • the radio frequency power applied to the target is less than 3000W , in a preferred embodiment, the radio frequency power applied to the target material is greater than or equal to 1000W and less than or equal to 2000W, wherein the ratio of the radio frequency power applied to the target material to the DC power applied to the target material is greater than or equal to 2, and less than or equal to 7,
  • the ratio is greater than or equal to 3 and less than or equal to 6, such as 3, 5, 6 and so on.
  • the setting of the above ratio helps to deposit a high-density, low-roughness film on the wafer surface, thereby improving the film quality.
  • the high-quality film surface can also inhibit the formation of a transition layer between the etching layer and the metal layer. , so that the oxidation of the metal layer can be reduced.
  • the radio frequency power applied to the base is less than 500W, and in a preferred embodiment, the radio frequency power applied to the base is greater than or equal to 50W and less than or equal to 200W.
  • FIG. 2 is a graph showing a comparison of the number of particle defects in oxide thin films prepared according to an embodiment of the present invention and the prior art.
  • FIG. 3 shows a comparison diagram of etching uniformity of oxide thin films prepared according to an embodiment of the present invention and the prior art. Referring to FIG. 2 and FIG. 3, it can be clearly seen that compared with the prior art, the particle defects of this technical solution are significantly reduced, the number of particles larger than 30 nanometers in the film on the wafer is less than 5, and at the same time, the uniformity of wet etching is also improved. This was greatly improved, with uniformity dropping from 12.49% to 2.24%.
  • step 2 DC power and radio frequency power are simultaneously applied to the target material, which can reduce the generation of particle defects during the oxide deposition process.
  • step 3 a second mixed gas of bombardment gas, oxidizing gas and nitrogen gas is introduced, and radio frequency power is applied to the susceptor, which can not only generate an oxynitride film in situ, but also perform certain etching on the surface of the oxide film. , so that the surface roughness of the oxide film can be reduced while reducing the surface defects of the oxide film.
  • step 4 the above-mentioned second mixed gas is continuously introduced, and at the same time, DC power and RF power are applied to the target material, and RF power is applied to the susceptor, so that high-density, low-roughness oxynitride can be deposited on the wafer surface. Therefore, the quality of the film can be improved, and the high-quality surface of the film can also inhibit the formation of a transition layer between the etching layer and the metal layer, thereby reducing the oxidation of the metal layer.
  • the method for preparing the oxide thin film provided by the embodiment of the present invention increases the control mode of ion energy and distribution during the thin film growth process, expands the process window, and provides an effective method for preparing high-density oxide thin film.

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Abstract

一种氧化物薄膜的制备方法，包括：步骤1：将待沉积薄膜的晶圆放入反应腔室的基座上；步骤2：向反应腔室内通入轰击气体和氧化气体的第一混合气体，对靶材施加直流功率和射频功率，激发第一混合气体形成等离子体，以轰击靶材在晶圆上形成氧化物薄膜；步骤3：停止对靶材施加直流功率和射频功率，向反应腔室内通入轰击气体、氧化气体和氮气的第二混合气体，对基座施加射频功率，激发第二混合气体形成等离子体，以轰击氧化物薄膜形成氮氧化物薄膜；步骤4：继续向反应腔室内通入第二混合气体，对靶材施加直流功率和射频功率，继续对基座施加射频功率，激发第二混合气体形成等离子体，以轰击靶材和步骤3形成的氮氧化物薄膜，以在步骤3形成的氮氧化物薄膜上形成氮氧化物薄膜。

Description

氧化物薄膜的制备方法 技术领域
本发明涉及半导体工艺领域，更具体地，涉及一种氧化物薄膜的制备方法。
背景技术
近年来，超大规模集成电路技术发展迅速，器件特征尺寸在不断缩小，器件密度在不断增大，金属化互连所带来的RC迟滞已经成为阻碍超高密度集成电路效能及速度的关键因素。因此，减少RC互连延迟成为近年来半导体行业的主攻方向。在集成电路制造工艺中，金属线通常嵌入在具有低介电常数的层间电介质(ILD)层之中。在大马士革工艺中，通常在层间电介质层和金属线上沉积蚀刻停止层，该蚀刻停止层用于在集成电路制造工艺的图案化制作过程中，保护位于蚀刻停止层所覆盖的材料在图案化期间不被蚀刻。该蚀刻停止层通常不会被完全去除，最终保留在制造的半导体器件中。
氧化铝因其良好的工艺兼容性逐渐被用作蚀刻停止层。制备氧化铝薄膜通常采用的一种方法是化学气相沉积(Chemical Vapor Deposition，以下简称CVD)方法，但是该CVD方法制备的薄膜杂质多、密度小且工艺成本高。还有一种是脉冲磁控溅射方法，该方法是一种物理气相沉积(Physical Vapor Deposition，以下简称PVD)方法，该PVD方法制备的氧化铝薄膜具有良好的薄膜均匀性、杂质少、密度大等优势，是目前集成电路金属化制程中最常用的方法之一。然而，在采用传统的PVD方法制备非导电氧化物薄膜时，会存在工艺窗口小、沉积速率低、蚀刻不均匀及频繁的电弧异常放电引起颗粒缺陷等问题，这些问题对后续工艺集成带来了很大的困难。因此，迫切需要寻找一种新的氧化物薄膜制备方法。
发明内容
本发明的目的是提出一种氧化物薄膜的制备方法，解决在工艺过程中沉积速率低、颗粒缺陷，表面粗糙度大，薄膜密度低的问题，所述制备方法包括：
步骤1：将待沉积薄膜的晶圆放入反应腔室的基座上；
步骤2：向所述反应腔室内通入轰击气体和氧化气体的第一混合气体，对靶材施加直流功率和射频功率，激发所述第一混合气体形成等离子体，以轰击所述靶材在所述晶圆上形成氧化物薄膜；
步骤3：停止对靶材施加直流功率和射频功率，向反应腔室内通入轰击气体、氧化气体和氮气的第二混合气体，对基座施加射频功率，激发第二混合气体形成等离子体，以轰击氧化物薄膜形成氮氧化物薄膜；
步骤4：继续向所述反应腔室内通入所述第二混合气体，对所述靶材施加直流功率和射频功率，继续对所述基座施加射频功率，激发所述第二混合气体形成等离子体，以轰击所述靶材和所述步骤3形成的所述氮氧化物薄膜，以在所述步骤3形成的氮氧化物薄膜上形成氮氧化物薄膜。
可选方案中，在所述步骤2中，对所述靶材施加的直流功率小于10000W，对所述靶材施加的射频功率小于3000W，其中，对所述靶材施加的射频功率与对所述靶材施加的直流功率的比值为大于等于2，且小于等于4。
可选方案中，在所述步骤2中，对所述靶材施加的直流功率为大于等于100W，且小于等于200W，对所述靶材施加的射频功率为大于等于300W，且小于等于600W，其中，对所述靶材施加的射频功率与对所述靶材施加的直流功率的比值为3。
可选方案中，在所述步骤4中，对所述靶材施加的直流功率小于10000W，对所述靶材施加的射频功率小于3000W，其中，对所述靶材施加的射频功率 与对所述靶材施加的直流功率的比值为大于等于2，且小于等于7。
可选方案中，在所述步骤4中，对所述靶材施加的直流功率为大于等于3000W，且小于等于6000W，对所述靶材施加的射频功率为大于等于1000W，且小于等于2000W，其中，对所述靶材施加的射频功率与对所述靶材施加的直流功率的比值为大于等于3，且小于等于6。
可选方案中，在所述步骤3和/或所述步骤4中，所述氧化气体和氮气的流量之和大于所述轰击气体的流量。
可选方案中，在所述步骤3和/或所述步骤4中，对所述基座施加的射频功率小于500W。
可选方案中，所述步骤1中的工艺条件为：所述反应腔室的真空度小于5×10-6Torr；所述基座的温度为大于等于250℃，且小于等于350℃。
可选方案中，在所述步骤2和/或所述步骤3中，所述轰击气体的流量小于500sccm，所述氧化气体的流量小于500sccm，其中，所述轰击气体的流量大于所述氧化气体的流量。
可选方案中，所述靶材包括铝、钛、硅、铪或钽靶材，或者包括铝、钛、硅、铪或钽的化合物靶材。
本发明的有益效果在于：
在步骤2中，对靶材同时施加直流功率和射频功率，能够减少氧化物沉积过程中颗粒缺陷的产生。在步骤3中，通入轰击气体、氧化气体和氮气的第二混合气体，并对基座施加射频功率，不仅可以原位生成氮氧化物薄膜，还可以对氧化物薄膜表面进行一定的刻蚀，从而可以在减少氧化物薄膜表面缺陷的同时降低表面的粗糙度。在步骤4中，继续通入上述第二混合气体，同时对靶材施加直流功率和射频功率，并对基座施加射频功率，可以在晶圆表面沉积形成高密度，低粗糙度的氮氧化物薄膜，从而可以提高薄膜质量，而且，高质量的薄膜表面还可以抑制在蚀刻层和金属层之间形成过渡层，从 而可以减少金属层的氧化。
本发明的方法具有其它的特性和优点，这些特性和优点从并入本文中的附图和随后的具体实施方式中将是显而易见的，或者将在并入本文中的附图和随后的具体实施方式中进行详细陈述，这些附图和具体实施方式共同用于解释本发明的特定原理。
附图说明
通过结合附图对本发明示例性实施例进行更详细的描述，本发明的上述以及其它目的、特征和优势将变得更加明显。
图1示出了根据本发明一实施例的氧化物薄膜的制备方法步骤流程图。
图2示出了根据本发明一实施例和现有技术制备的氧化物薄膜颗粒缺陷数量的对比图。
图3示出了根据本发明一实施例和现有技术制备的氧化物薄膜刻蚀均匀性的对比图。
具体实施方式
下面将更详细地描述本发明。虽然本发明提供了优选的实施例，然而应该理解，可以以各种形式实现本发明而不应被这里阐述的实施例所限制。相反，提供这些实施例是为了使本发明更加透彻和完整，并且能够将本发明的范围完整地传达给本领域的技术人员。
本发明一实施例提供了一种氧化物薄膜的制备方法，图1示出了根据本发明一实施例的氧化物薄膜的制备方法步骤流程图。请参考图1，氧化物薄膜的制备方法包括：
步骤1：将待沉积薄膜的晶圆放入反应腔室的基座上；
步骤2：向反应腔室内通入轰击气体和氧化气体的第一混合气体，对靶材施加直流功率和射频功率，激发该第一混合气体形成等离子体，以轰击靶 材在晶圆上形成氧化物薄膜；
步骤3：停止对靶材施加所述直流功率和射频功率，向反应腔室内通入轰击气体、氧化气体和氮气的第二混合气体，对基座施加射频功率，激发第二混合气体形成等离子体，以轰击氧化物薄膜形成氮氧化物薄膜；
步骤4：继续向反应腔室内通入上述第二混合气体，对靶材施加直流功率和射频功率，继续对基座施加射频功率，激发第二混合气体形成等离子体，以轰击靶材和上述步骤3形成的氮氧化物薄膜，以在上述步骤3形成的氮氧化物薄膜上形成氮氧化物薄膜。
为了便于理解本方案，首先对用于制备薄膜的设备进行简单的介绍。薄膜的制备在反应腔室中进行，反应腔室中设有基座，用于承载待沉积薄膜的晶圆，该基座具备加热和/或冷却功能，以能够对晶圆的温度进行控制。反应腔室连接有真空***，该真空***可对反应腔室进行抽气，以使反应腔室达到所需的真空度，以满足工艺所需的真空条件。工艺所需的气体(如轰击气体、氧化气体等)通过进气管路通入反应腔室，且该进气管路上可以设置流量计，以控制气体的流量。工艺所需的靶材被密封在反应腔室的上方区域(基座的上方)。上述靶材可以是纯金属也可以是金属化合物，也可以是硅或二氧化硅(当需要沉积硅的氧化物)。进行薄膜沉积时，电源会施加功率至靶材，使其相对于接地的反应腔室为负偏压，另外，高压使轰击气体、氧化气体电离放电而产生带正电的等离子体，带正电的等离子体被靶材吸引并轰击靶材。当等离子体的能量足够高时，会使靶材表面的原子逸出并沉积在晶圆上，以实现在晶圆表面上沉积薄膜。
本实施例以在晶圆表面沉积氧化铝和氮氧化铝的复合薄膜为例，对氧化物薄膜的制备方法进行详细说明。
具体地，执行步骤1，根据沉积的薄膜不同，对反应腔室设定适合的工艺条件，将待沉积薄膜的晶圆放入反应腔室的基座上，将基座温度调至工艺 所需的温度。在本实施例中，制备方法用于沉积氧化铝薄膜，在这种情况下，设定的工艺条件为，反应腔室的真空度小于5×10 -6Torr；基座的温度为大于等于250℃，且小于等于350℃，优选的，如300℃。
执行步骤2，向反应腔室内通入轰击气体和氧化气体的第一混合气体，对靶材施加直流功率和射频功率，激发该第一混合气体形成等离子体，以轰击靶材在晶圆上形成氧化物薄膜。
在现有技术中，对靶材只施加脉冲直流功率，由于氧化铝薄膜是一种非导电氧化物，脉冲直流功率在一个周期内存在正电压和负电压两个阶段，在负电压阶段，直流电源在靶材上加载负电压，此时等离子体会轰击靶材，实现靶材的溅射；在正电压阶段，直流电源在靶材上加载正电压，此时会向靶材引入电子，以中和靶材表面累积的正电荷。这种脉冲直流功率的加载方式会导致工艺过程中沉积速率低、蚀刻不均匀、因频繁的电弧异常放电引起颗粒缺陷，薄膜表面粗糙度大，薄膜密度低，容易吸附空气中的水、氧、碳等杂质气体形成表面缺陷等的问题，对后续工艺集成造成了很大的困难。
为了解决上述问题，本实施例的步骤2中，对靶材同时施加直流功率和射频功率，这种射频/直流共溅射的功率加载方式可以在靶材上形成负电压，从而可以促进等离子体轰击靶材，实现靶材的溅射。这种射频/直流共溅射的功率加载方式还可以降低离子能量，避免对晶圆底层的层间介质(ILD)薄膜造成损伤，从而可以形成高密度的氧化铝薄膜(例如用作接触层)，此外，还可以减少金属氧化物沉积过程中的颗粒缺陷的产生，同时可以在沉积氮氧化物薄膜的过程中，抑制空气中的水、氧、碳在金属氧化物表面吸附产生颗粒缺陷。另外，靶材上增加射频功率，可以增加等离子体中氧的碰撞离化，改变氧原子的分布，改善氧化物薄膜湿法蚀刻均匀性问题。
执行步骤3，停止对靶材施加直流功率和射频功率，向反应腔室内通入轰击气体、氧化气体和氮气的第二混合气体，对基座施加射频功率，激发第 二混合气体形成等离子体，以轰击氧化物薄膜形成氮氧化物薄膜。
在本步骤中，对基座施加射频功率，可以在基座上形成负偏压，以吸引等离子体轰击薄膜表面，从而达到对步骤2形成的氧化物薄膜的表面进行处理的目的，这种表面处理可以原位形成氮氧化物薄膜，即在氧化物薄膜的表面生成一层较薄的氮氧化物薄膜，以减少氧化物薄膜表面缺陷；同时，上述表面处理还可以对形成的氧化物薄膜表面进行一定的刻蚀，以降低薄膜表面的粗糙度。
执行步骤4，继续向反应腔室内通入上述第二混合气体，对靶材施加直流功率和射频功率，继续对基座施加射频功率，激发第二混合气体形成等离子体，以轰击靶材和上述步骤3形成的氮氧化物薄膜，以在上述步骤3形成的氮氧化物薄膜(或者说氧化物薄膜)上形成氮氧化物薄膜。
在本步骤中，同时对靶材施加直流功率和射频功率，并对基座施加射频功率，可以同时对薄膜进行刻蚀和沉积，且沉积的速率大于刻蚀的速率，以能够在晶圆表面沉积形成高密度，低粗糙度的薄膜，从而可以提高薄膜质量，而且，高质量的薄膜表面还可以抑制在蚀刻层和金属层之间形成过渡层，从而可以减少金属层的氧化。
在一些可选的实施例中，在步骤2中，轰击气体例如为氩气，氧化气体例如为氧气。
在一些可选的实施例中，在步骤2中，反应腔室的工艺压力维持在大于等于3mTorr，且小于等于10mTorr。
在一些可选的实施例中，在步骤2中，轰击气体的流量小于500sccm，优选实施例中，轰击气体的流量大于等于50sccm，且小于等于200sccm；氧化气体的流量小于500sccm，优选实施例中，氧化气体的流量大于等于20sccm，且小于等于100sccm。其中，轰击气体的流量大于氧化气体的流量，即轰击气体与氧化气体的比例大于1。这和现有技术(轰击气体与氧化气体 的比例小于0.5)有很大的不同，即，本实施例相对于现有技术减小了氧化气体的占比，这样可以避免氧化气体的占比过高，氧化气体的占比过高不利于颗粒缺陷和蚀刻均匀性的控制，还可以减少金属氧化物沉积过程中的颗粒缺陷的产生，同时可以在沉积氮氧化物薄膜的过程中，抑制空气中的水、氧、碳在金属氧化物表面吸附产生颗粒缺陷。
在一些可选的实施例中，在步骤2中，对靶材施加的直流功率小于10000W，优选实施例中，该直流功率大于等于100W，且小于等于200W。对靶材施加的射频功率小于3000W，优选实施例中，射频功率大于等于300W，且小于等于600W。其中，对靶材施加的射频功率与对靶材施加的直流功率的比值大于等于2，且小于等于4，优选实施例中，该比值为3。通过将上述比值设定在该数值范围内，能够在沉积氧化铝薄膜时，增加铝和氧的原子在高密度等离子体中的离化和碰撞，改变薄膜在衬底表面生长时的横向迁移，从而形成低损伤、高密度薄膜，避免对底层的低介电常数的层间介质层造成损伤，改变材料的介电常数。
在一些可选的实施例中，在步骤3中，轰击气体例如为氩气，氧化气体例如为氧气。上述氮气在离化后用于对形成的氧化物薄膜表面起到一定的轰击作用。
在一些可选的实施例中，在步骤3中，反应腔室的工艺压力维持在大于等于3mTorr，且小于等于10mTorr。
在一些可选的实施例中，在步骤3中，轰击气体的流量小于500sccm，优选实施例中，轰击气体的流量范围大于等于50sccm，且小于等于200sccm；氧化气体的流量小于500sccm，优选实施例中，氧化气体的流量大于等于20sccm，且小于等于100sccm。其中，氧化气体和氮气的流量之和大于轰击气体的流量，即，氧化气体和氮气的流量之和与轰击气体的流量的比值大于1。这样设置，有助于对形成的氧化物薄膜表面进行一定的刻蚀，以降低薄膜 表面的粗糙度。
在一些可选的实施例中，在步骤3中，对基座施加的射频功率小于500W，优选实施例中，对基座施加的射频功率范围为大于等于50W，且小于等于100W。
在一些可选的实施例中，在步骤4中，反应腔室的工艺压力维持在大于等于3mTorr，且小于等于10mTorr。
在一些可选的实施例中，在步骤4中，轰击气体的流量小于500sccm，优选实施例中，轰击气体的流量大于等于50sccm，且小于等于200sccm；氧化气体的流量小于500sccm，优选实施例中，氧化气体的流量大于等于20sccm，且小于等于100sccm。其中，轰击气体的流量大于氧化气体的流量，即轰击气体与氧化气体的比例大于1。
在一些可选的实施例中，在步骤4中，对靶材施加的直流功率小于10000W，优选实施例中，该直流功率大于等于3000W，且小于等于6000W；对靶材施加的射频功率小于3000W，优选实施例中，对靶材施加的射频功率大于等于1000W，且小于等于2000W，其中，对靶材施加的射频功率与对靶材施加的直流功率的比值大于等于2，且小于等于7，优选的，该比值大于等于3，且小于等于6，如3、5、6等。上述比值的设置，有助于在晶圆表面沉积形成高密度，低粗糙度的薄膜，从而可以提高薄膜质量，而且，高质量的薄膜表面还可以抑制在蚀刻层和金属层之间形成过渡层，从而可以减少金属层的氧化。
在一些可选的实施例中，在步骤4中，对基座施加的射频功率小于500W，优选实施例中，对基座施加的射频功率大于等于50W，且小于等于200W。
图2示出了根据本发明一实施例和现有技术制备的氧化物薄膜颗粒缺陷数量的对比图。图3示出了根据本发明一实施例和现有技术制备的氧化物薄膜刻蚀均匀性的对比图。参考图2和图3，可以清楚的看到本技术方案相对 于现有技术，颗粒缺陷明显减少，晶圆上膜内大于30纳米的颗粒数量在5颗以内，同时，湿法蚀刻均匀性也得到了极大的改善，均匀性从12.49％降到2.24％。
以上描述以形成铝的氧化物和氮氧化物薄膜为例，应该理解本发明的方法还可以制备其他薄膜，如用于制备钛、硅、铪或钽的氧化物和氮氧化物的复合薄膜。
综上所述，本发明实施例提供的氧化物薄膜的制备方法，在步骤2中，对靶材同时施加直流功率和射频功率，能够减少氧化物沉积过程中颗粒缺陷的产生。在步骤3中，通入轰击气体、氧化气体和氮气的第二混合气体，并对基座施加射频功率，不仅可以原位生成氮氧化物薄膜，还可以对氧化物薄膜表面进行一定的刻蚀，从而可以在减少氧化物薄膜表面缺陷的同时降低表面的粗糙度。在步骤4中，继续通入上述第二混合气体，同时对靶材施加直流功率和射频功率，并对基座施加射频功率，可以在晶圆表面沉积形成高密度，低粗糙度的氮氧化物薄膜，从而可以提高薄膜质量，而且，高质量的薄膜表面还可以抑制在蚀刻层和金属层之间形成过渡层，从而可以减少金属层的氧化。另外，本发明实施例提供的氧化物薄膜的制备方法，其增加了薄膜生长过程中离子能量和分布的控制方式，扩大了工艺窗口，为制备高密度氧化物薄膜提供了一种有效方法。
以上已经描述了本发明的各实施例，上述说明是示例性的，并非穷尽性的，并且也不限于所披露的各实施例。在不偏离所说明的各实施例的范围和精神的情况下，对于本技术领域的普通技术人员来说许多修改和变更都是显而易见的。

Claims (10)

  1. 一种氧化物薄膜的制备方法，其特征在于，所述方法包括：
    步骤1：将待沉积薄膜的晶圆放入反应腔室的基座上；
    步骤2：向所述反应腔室内通入轰击气体和氧化气体的第一混合气体，对靶材施加直流功率和射频功率，激发所述第一混合气体形成等离子体，以轰击所述靶材在所述晶圆上形成氧化物薄膜；
    步骤3：停止对所述靶材施加所述直流功率和射频功率，向所述反应腔室内通入轰击气体、氧化气体和氮气的第二混合气体，对所述基座施加射频功率，激发所述第二混合气体形成等离子体，以轰击所述氧化物薄膜形成氮氧化物薄膜；
    步骤4：继续向所述反应腔室内通入所述第二混合气体，对所述靶材施加直流功率和射频功率，继续对所述基座施加射频功率，激发所述第二混合气体形成等离子体，以轰击所述靶材和所述步骤3形成的所述氮氧化物薄膜，以在所述步骤3形成的氮氧化物薄膜上形成氮氧化物薄膜。
  2. 根据权利要求1所述的方法，其特征在于，在所述步骤2中，对所述靶材施加的直流功率小于10000W，对所述靶材施加的射频功率小于3000W，其中，对所述靶材施加的射频功率与对所述靶材施加的直流功率的比值为大于等于2，且小于等于4。
  3. 根据权利要求2所述的方法，其特征在于，在所述步骤2中，对所述靶材施加的直流功率为大于等于100W，且小于等于200W，对所述靶材施加的射频功率为大于等于300W，且小于等于600W，其中，对所述靶材施加的射频功率与对所述靶材施加的直流功率的比值为3。
  4. 根据权利要求1所述的方法，其特征在于，在所述步骤4中，对所 述靶材施加的直流功率小于10000W，对所述靶材施加的射频功率小于3000W，其中，对所述靶材施加的射频功率与对所述靶材施加的直流功率的比值为大于等于2，且小于等于7。
  5. 根据权利要求4所述的方法，其特征在于，在所述步骤4中，对所述靶材施加的直流功率为大于等于3000W，且小于等于6000W，对所述靶材施加的射频功率为大于等于1000W，且小于等于2000W，其中，对所述靶材施加的射频功率与对所述靶材施加的直流功率的比值为大于等于3，且小于等于6。
  6. 根据权利要求1所述的方法，其特征在于，在所述步骤3和/或所述步骤4中，所述氧化气体和氮气的流量之和大于所述轰击气体的流量。
  7. 根据权利要求1所述的方法，其特征在于，在所述步骤3和/或所述步骤4中，对所述基座施加的射频功率小于500W。
  8. 根据权利要求1所述的方法，其特征在于，所述步骤1中的工艺条件为：所述反应腔室的真空度小于5×10 -6Torr；所述基座的温度为大于等于250℃，且小于等于350℃。
  9. 根据权利要求1所述的方法，其特征在于，在所述步骤2和/或所述步骤3中，所述轰击气体的流量小于500sccm，所述氧化气体的流量小于500sccm，其中，所述轰击气体的流量大于所述氧化气体的流量。
  10. 根据权利要求1-9任一项所述的方法，其特征在于，所述靶材包括铝、钛、硅、铪或钽靶材，或者包括铝、钛、硅、铪或钽的化合物靶材。
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