Method of preparing thin-film metal structure of tungsten on silicon

FIELD: physics; conductors.

SUBSTANCE: invention relates to semiconductor micro- and nanoelectronics and can be used in making integrated circuits, in making electrodes in transistors and capacitor plates, in making contacts and conduction regions on a silicon surface, as conducting, thermostable and barrier layers in metallisation systems. The method of making a thin-film metal structure of tungsten on silicon involves making a nanometer sublayer of an adhesion promoter on a silicon substrate and subsequent deposition of a thin film of tungsten through gas-phase chemical deposition through reduction of tungsten hexafluoride with hydrogen at low pressure. The adhesion promoter used is tungsten silicide W5Si3.

EFFECT: invention improves quality of the obtained metal structure of tungsten on silicon with simplification of the process at the same time.

3 cl, 1 dwg, 3 ex

 

The invention relates to a semiconductor micro - and nanoelectronics and can be used in the manufacture of integrated circuits (ICS): when forming the electrodes in the transistors and plates of a capacitor, the formation of the contacts and conductive areas on the silicon surface as a conductive, thermally stable and barrier layers in metallization systems. Gas-phase chemical deposition (CVD) of tungsten is the main process of multilevel positive opening operation metallization due to good conformity coatings.

A known method of manufacturing a thin film metal structure of tungsten on silicon, including thin film deposition of tungsten on silicon CVD method on reduction reaction of tungsten hexafluoride with hydrogen in the reactor low pressure activation of hydrogen [Malikov IV, ivy SV, Shapoval HE "Vapor deposition of thin films of tungsten with HF activation, high-purity substances, 1991, No. 4, s-182].

However, all the positive properties of tungsten metallization (tungsten is not susceptible to electromigration resistant to thermal stress, high thermal stability, low activity of oxidation, good conductivity and other) films of tungsten have low structural integrity and often peel off due to poor adhesion of tungsten to amnio, which makes their practical use in IC technology.

A known method of manufacturing a thin film metal structure of tungsten on silicon adopted for the prototype [Handbook of semiconductor manufacturing technology/ ed. Y.Nishi, R.Doering, Marcell Dekker Inc., N.Y., USA, 2000, p.342-345]. The method comprises applying a thin film of tungsten by the method of gas-phase chemical deposition by reduction reaction of tungsten hexafluoride with hydrogen in the reactor low pressure activation of hydrogen on a substrate made of silicon covered with nanometer sublayer of the adhesion promoter. As the promoter used a titanium nitride with a thickness of 30-50 nm to improve the adhesion of a film of tungsten to silicon. Applying a film of titanium nitride (TiN) is an independent process, which is included as an additional step in the overall process flow and requires expensive equipment. To obtain TiN films used processes reactive magnetron sputtering or by collimation or ionization of the sputtered particles.

However, the quality of the resulting structures do not always meet the requirements of modern technology. The formation of TiN sublayer associated with the use of additional reagents, which may be undesirable in IC technology, as any reagent potential source of contamination and unpredictable sources of interference. In addition to TiN, stage zarodysheobrazovanie is additionally injected silane (SiH 4), which further complicates the process.

The presented invention solves the problem of improving the quality of the metal structure of tungsten on silicon with simultaneous simplification of the process.

The technical effect is to obtain integral and stable heterostructures due to the formation of nanoscale sub-layer of the silicide of tungsten (W5Si3) high density. In addition, there is a simplification of the process by combining in a single process stages receiving sublayer of the promoter and the tungsten film.

This object is achieved by a method of manufacturing a thin film metal structure of tungsten on silicon, including the creation of nanoscale sub-layer of the adhesion promoter, followed by the application of a thin film of tungsten by the method of gas-phase chemical deposition by reduction reaction of tungsten hexafluoride with hydrogen on a substrate of silicon under reduced pressure. The novelty of the method lies in the fact that, as the adhesion promoter is used, the tungsten silicide W5Si3.

The silicide W5Si3is structured according to both the tungsten and silicon, has a high perfection of the interface film-substrate interface, which makes it a good adhesive about oterom tungsten to silicon. In addition, the dense structure of the silicide W5Si3prevents the formation of other silicides with higher silicon content and lower conductivity.

The sublayer silicide of tungsten W5Si3can be obtained by any means.

The most technologically advanced creation sublayer of tungsten silicide to carry out the processing of the silicon substrate before deposition of a film of tungsten pairs of tungsten hexafluoride in the same reactor at a temperature of 100-200°C for 10-20 minutes. Under these conditions, a thin surface layer of active silicon and a favorable ratio of tungsten to silicon leads to the formation of stable thick silicide film permanent makeup W5Si3that is a diffusion barrier for tungsten hexafluoride and silicon, which leads to the termination of the reaction siliconware. The result is a self-limited layer of silicide W5Si3thickness of ~20 nm with a high conductivity, which ensures good adhesion of the tungsten.

The best option CVD process is the vapor deposition of tungsten by reduction reaction of tungsten hexafluoride with hydrogen using an RF-activated hydrogen at temperatures between 200°C and more.

The use of HF-activated hydrogen in the process gas-phase chemical is Sardinia allows to reduce the process temperature to room. The temperature reduction is an important condition for the formation of contacts to the semiconductor layers, especially at the nanoscale. However, under these conditions, high-quality film can be obtained only at temperatures higher than 200°C.

On the proposed technology obtained thin film of tungsten with a thickness of about 100 nm and a resistivity of 8×10-6Ohm×cm, close to the resistance of the bulk metal.

The drawing shows a General view of the installation for the manufacture of thin film metal structure of tungsten on silicon.

The installation consists of the following main parts: quartz reactor 1, the furnace of resistance 2 with controlled heating and precise temperature maintenance with the help of art, a silicon wafer 3, the vacuum system 4, including nitrogen pump, booster pump and pump type "Ruts" with control devices vacuum "W-2" and "EDC-1", the source of tungsten hexafluoride with 5 valve fine adjustment and a pressure sensor, supply system and hydrogen purification 6 "Palladium of 0.5 for hydrogen purification by filtration through palladium filters, inductor RF generator 7 with a frequency of 13.56 MHz and a power of 500 watts to excite the plasma, the pressure sensor 8 for controlling the pressure of the gas mixture in the reactor, the system load 9.

As a source of tungsten used clean the th tungsten hexafluoride, corresponding to THE 6-02-18-137-87.

As the substrate used in the plate resistance of silicon orientation <100>.

Pre substrate of silicon processed pairs of tungsten hexafluoride within 10-20 minutes at a temperature of 100-200°C.

Deposition of tungsten is carried out under reduced pressure, varying the temperature from 200 to 500°C depending on the type of CVD process. In normal mode CVD process takes place at temperatures above 350°C. To reduce the temperature of the film deposition of the tungsten used the activation of hydrogen, which allows to obtain high-quality films at temperatures higher than 200°C.

The higher the process temperature is undesirable in the technology of forming integrated circuits, because they lead to more poorly controlled sources of structural damage

Measurement of the thickness of the films was carried out on the Talystep profilometer. The resistivity of the films was measured chetyrehsetovom contact method.

The study of the chemical interactions of the surface layers of the silicon substrate with a film of tungsten was performed by the method of thin-film x-ray diffractometry.

The surface condition of the sample was controlled using atomic force microscopy (atomic force microscope AFM R-04).

Besides visually controlled visible defects and violation of the integrity of dormancy is itia.

These examples suggest, but do not limit the invention.

Example 1.

Obtaining thin films of tungsten rebuilding its hexafluoride with hydrogen was carried out in the installation shown in the drawing.

In a quartz reactor (1) was placed pedestal with silicon plates (3) with an area of 1.5×1.5 cm2. The maximum number of simultaneously processed silicon wafer 10 pieces. Using system degassing (4) brought the pressure up to 0.13 PA. Opened the valve on the feeder WF6(5) and created the pressure in the reactor 10 PA. Before performing a CVD process prior to the deposition of tungsten films on silicon substrate was treated with pairs of tungsten hexafluoride supplied from the system (5) for 15 minutes at 200°C, supported by high precision temperature controller (2). This forms the active silicon layer. Which leads to the formation of a silicide of tungsten W5Si3high density (14.523 g/cm3). This silicide is a barrier to further penetration of tungsten hexafluoride, and the reaction siliconware stopped and formed a self-silicide sublayer W5Si3thickness of ~20 nm.

Then spent the vapor deposition of the tungsten film. In the reactor (1) from the system (6) was applied to the hydrogen, which passed clean through palladium Phi is try. The total pressure in the reactor brought up to 53.2 PA. The temperature of the process was 400°C. the duration of the deposition process was determined by the desired thickness adjusting film of tungsten.

The resistivity of the obtained films of tungsten with a thickness of 150 nm was more close to the resistance of the bulk metal and was 8×10-6Ohm·see

Visual inspection with a microscope showed no violations of the integrity of the coating and visible defects.

Nuclear microscopy measurements showed a uniform coating over the whole surface of the substrate. The film is solid, and the average roughness with film thickness of 100 nm was at the level of 8-12 nm.

Example 2. Same as in example 1, except that the vapor deposition of tungsten by reduction reaction of tungsten hexafluoride with hydrogen was performed using an RF-activated hydrogen. The temperature vapour deposition of tungsten was 100°C.

The obtained film of tungsten at the same coating thickness (150 nm)had a higher specific resistance 62×10-6Ohm·cm, which makes them unsuitable for the task.

Example 3. Same as in example 2, only the vapor deposition of tungsten by reduction reaction of tungsten hexafluoride with hydrogen using an RF-activated hydrogen was carried out at pace is the atur 200°C.

The resistivity of the obtained films of tungsten with a thickness of 150 nm was close to the resistance of the bulk metal and declined to a value of 11×10-6Ohm·see

Visual inspection with a microscope showed no violations of the integrity of the coating and visible defects.

Nuclear microscopy measurements showed a uniform coating over the whole surface of the substrate, the average roughness with film thickness of 150 nm was at the level of 8-12 nm.

Thus, the use of RF-activated hydrogen is possible to reduce the temperature of the CVD process at 200°C.

As follows from the above, the present invention allows to create nanometer sublayer of the adhesion promoter of the tungsten silicide composition W5Si3high density 14.523 g/cm3, while the density of the adhesion promoter in the prototype TiN 5.44 g/cm3. That, in turn, allows to obtain a stable thin-film metal structure of tungsten on silicon with a high conductivity, good adhesion and structural integrity, good reflectivity and thermal stability. The resistivity of the obtained thin films of tungsten approached the resistance of the bulk metal (5,5×10-6Ohm·cm) and was 8×10-6Ohm·see

1. A method of manufacturing a thin-film metal is tructure tungsten on silicon, including the creation of nanoscale sub-layer of the adhesion promoter, followed by the application of a thin film of tungsten by the method of gas-phase chemical deposition by reduction reaction of tungsten hexafluoride with hydrogen on a substrate of silicon under reduced pressure, characterized in that the adhesion promoter is used, the tungsten silicide W5Si3.

2. The method according to claim 1, characterized in that to create a sub-layer of tungsten silicide before applying the film of tungsten silicon wafer treated with pairs of tungsten hexafluoride in the same reactor at a temperature of 100-200°C for 10-20 minutes

3. The method according to claim 1, characterized in that the gas-phase chemical deposition is carried out with the activation of hydrogen at a temperature more than 200°C.



 

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