TW201319316A - Method of upgrading material at low temperature and its processing device - Google Patents

Abstract

A method of upgrading a material at low temperature comprises a first supercritical fluid cleaning step, an isothermal processing step, and a second supercritical fluid cleaning step. The first supercritical fluid cleaning step comprises placing a material to be processed in a vacuum environment and then cleaning the material to be processed with supercritical fluid. The isothermal processing step comprises exposing the cleaned material to be processed to an environment with a pressure of 70-400 atm and a temperature of 100-450 DEG C. The second supercritical fluid cleaning step comprises using supercritical fluid to clean the material to be processed after the isothermal processing step. Therefore, the isothermal processing step is carried out at a low temperature and high pressure environment to make the material to be processed under the experience fine granulation and recrystallization to obtain a high quality material with excellent uniformity and coverage. This invention also provides a processing device for upgrading a material at low temperature.

Description

Low-temperature material quality method and processing device thereof

The invention relates to a method for improving the quality of a material and a device thereof, in particular to a method and a device for improving the quality of a material by a low temperature and high pressure method.

In the existing semiconductor and electronic product processing and production processes, most of them are deposited by physical vapor deposition (PVD), arc physical vapor deposition (PVD), or chemical vapor deposition (Chemical Vaper Deposition). A thin film is deposited on a substrate, and the pattern to be formed is transferred onto the substrate by using Lithography and Etching techniques and the desired three-dimensional structure is stacked.

The quality of the electronic products produced by the above method largely determines whether the quality of the film formed during the deposition process is good or not, and whether the static charge and the dirt accumulated on the semi-finished product in the process are completely removed. In the existing process, when the semi-finished product is deposited in a vacuum environment, it is necessary to break the vacuum and move to a high-temperature furnace tube machine, and then access the machine with a high-temperature ambient gas (Ambient gas) of more than 1000 degrees Celsius. The semi-finished product formed by the film is subjected to an anneaal treatment to uniformize the grain structure inside the material.

However, when the film material is treated at a high temperature for a long time, there is a problem that thermal stress is accumulated in the produced film, and the thermal stress will have a serious influence on the reliability of the final product, and the industry has an increasingly strict line width requirement. The existing technology that uses high temperature and long-term constant temperature treatment to obtain high-quality thin films will be gradually eliminated, and in future electronic products such as soft electronics and flexible electronics, which are highly demanding in reliability, they may not continue to be applied. .

In addition, the existing process technology can not provide a complete and effective solution to the problem of accumulation of dirt and static charge in the process. This problem is bound to be more stringent in the trend of online width and reliability of finished products. Yield and reliability have a considerable impact.

Accordingly, it is an object of the present invention to provide a treatment method for improving the quality of a film material at a relatively low temperature.

Therefore, the method for improving the quality of the low temperature material of the present invention comprises a first supercritical fluid cleaning step, a constant temperature treatment step, and a second supercritical fluid cleaning step.

The first supercritical fluid cleaning step is to first place a material to be treated in a vacuum environment, and then clean the material to be treated with a fluid in a supercritical state.

The constant temperature treatment step is to expose the material to be treated which has been cleaned by the first supercritical fluid cleaning step to an environment having a pressure of 70 to 400 atm and a temperature of 100 to 450 degrees Celsius.

The second supercritical fluid cleaning step is to clean the material to be treated that has passed through the thermostatic treatment step with a fluid in a supercritical state.

Another object of the present invention is to provide a low-temperature material quality processing apparatus suitable for performing the high-quality method of the low-temperature material, comprising a body, a processing unit disposed in the body, and a deposition disposed in the body The unit, a transport unit disposed in the body, and a fluid unit disposed in the body.

An accommodating space is formed in the body, the processing unit is located in the accommodating space of the body and has a processing chamber, and the temperature and pressure in the processing chamber are adjustable. The deposition unit is located in the accommodating space of the body and has a deposition chamber, and is capable of plating a film on the surface of the material to be processed. The conveying unit is located in the accommodating space of the body and carries the material to be processed, and is accessed in the processing unit and the deposition unit according to a preset process. The fluid unit is in communication with the processing chamber of the processing unit and is capable of controlling a fluid flow into the processing chamber.

The effect of the present invention is to use a constant temperature treatment in a relatively low temperature and a relatively high pressure environment to fine-grain and recrystallize the material to be treated to obtain uniformity (Uniformity) and coverage (Step). Coverage) Good quality materials. In addition, it is also possible to convert the film with the original quality unevenness or low cost into a fine film of high quality film (Thin Film) for the subsequent process.

The above and other technical features, features, and advantages of the present invention will be apparent from the following detailed description of the preferred embodiments.

Before the present invention is described in detail, it is noted that in the following description, similar elements are denoted by the same reference numerals.

Referring to FIG. 1, a first preferred embodiment of the method for improving the quality of a low temperature material of the present invention comprises a first supercritical fluid cleaning step 1, a constant temperature processing step 2, and a second supercritical fluid cleaning step 3.

The first supercritical fluid cleaning step 1 is to first place a material to be treated in a vacuum environment, and then clean the material to be treated with a fluid in a supercritical state. In actual implementation, the material to be treated is placed in a closed space, and the space is evacuated, and then the fluid is introduced into the space, and it is confirmed that a predetermined amount of fluid has passed into the space. After that, the pressure and temperature in the space are adjusted, and the target value of the adjustment is the critical condition of the fluid. In this embodiment, graphite is used as the material to be treated, and carbon dioxide is used as the fluid, so the temperature and pressure in the space should be increased to at least 31.1 degrees Celsius (°C) and 72.8 atmospheres (atm), respectively. Of course, other types of fluids can also be used, such as nitrous oxide (critical temperature 36.4 ° C, critical pressure 72.5 atm), trifluorochloromethane (critical temperature 28.8 ° C, critical pressure 38.7 atm), difluoromethylene chloride ( The critical temperature is 111.7 ° C and the critical pressure is 37.4 atm. It is only necessary to adjust the temperature and pressure in the space to the corresponding critical conditions, depending on the actual situation.

Using the first supercritical fluid cleaning step 1 to operate the fluid under the operating conditions of its critical conditions to bring the fluid into a supercritical state, and the fluid in the supercritical state has a very high solubility, and can be dissolved and adhered. Contamination, particles, and static charges on the surface of the object to be treated, thereby effectively removing contaminants on the surface of the material to be treated, so that the material to be treated can be cleaned under conditions The next process flow.

Referring to FIG. 1 , in the thermostatic treatment step 2, the material to be treated after being cleaned by the first supercritical fluid cleaning step 1 is exposed to an environment having a pressure of 70 to 400 atm and a temperature of 100 to 450 degrees Celsius. . In actual implementation, the temperature and pressure conditions in the space are further increased to 100-450 ° C and 70-400 atm, respectively. In this embodiment, the operating conditions are the temperature of 180 ° C and the pressure of 200 atm. The object to be treated was subjected to a constant temperature treatment for 3 hours.

Through the constant temperature treatment in the low temperature and high pressure state, the material to be treated can be subjected to a process of fine graining (Grain) and recrystallization (Recrystallization), thereby achieving high-quality materials with high grain uniformity and coverage.

Referring to Fig. 2 to Fig. 4, Fig. 2 is a photomicrograph of the electron microscope before treatment, and Figs. 3 and 4 are photomicrographs (different magnifications) of the electron microscope after being treated at a constant temperature of 180 ° C and 200 atm for 3 hours. It can be seen from Fig. 3 and Fig. 4 that after 3 hours of low temperature and high pressure constant temperature treatment, the grain structure of the material to be treated (graphite) has changed from a spherical shape with a different particle size before treatment to a uniform size. The lattice shape is arranged neatly, so that the overall uniformity of the material is higher, and the gap between the crystal grains and the crystal grains is also greatly reduced, and the density and overall coverage of the material can be greatly improved.

It should be noted that the constant temperature processing step 2 of the embodiment is processed at a constant temperature (180 ° C) and a pressure (200 atm), but in fact, the temperature and pressure of the constant temperature treatment step 2 may also vary with time, for example In the constant temperature step, the material to be treated may be subjected to a constant temperature treatment for 1.5 hours at an operating condition of 180 ° C and 200 atm, and then the material to be treated is subjected to constant temperature treatment for 1 hour at an operating condition of 250 ° C and 100 atm. Finally, the material to be treated is subjected to a constant temperature treatment at 180 ° C and 200 atm for 1 hour, so that a finished product having higher grain density and overall coverage can be obtained, but it should be noted that the above processing time And the corresponding working conditions are only used for the specific material to be treated (in the present embodiment, graphite), and the actual implementation depends on the material to be treated to be processed, and is not limited herein.

Referring back to FIG. 1, after the constant temperature treatment step 2 is completed, the second supercritical fluid cleaning step 3 is performed. In the second supercritical fluid cleaning step 3, the material to be treated that has passed through the thermostatic treatment step 2 is cleaned by a fluid in a supercritical state. In this embodiment, the second supercritical fluid cleaning step 3 is The operation mode and conditions are the same as those of the first supercritical fluid cleaning step 1, and the functions and effects thereof are also the same, and thus will not be described herein.

The main object of the first preferred embodiment of the present invention is to re-quality the material to be processed which is to be further improved in quality, for example, if the material to be treated has been annealed (may not be annealed yet) Processing), but the finished product or the grain quality of the film formed thereon is not good, or there are fine cracks on the surface, and the method of the embodiment can be used to re-quality the material to be treated twice to obtain The grain structure with better density and overall coverage, even repairing the existing fine cracks.

Referring to FIG. 5, a second preferred embodiment of the method for improving the quality of the low temperature material of the present invention is substantially the same as that of the first preferred embodiment. The difference is that the second preferred embodiment further includes a first The deposition step 4 between the critical fluid cleaning step 1 and the constant temperature treatment step 2 is to form a film on the surface of the material to be treated after the first supercritical fluid cleaning step 1 is cleaned. In this embodiment, the film is formed by chemical vapor deposition, but may also be formed by sputtering, sintering, physical vapor deposition, arc physical vapor deposition, or electron cyclotron resonance chemical vapor deposition. The film is deposited on the surface of the material to be treated, depending on actual needs.

The main purpose of the second preferred embodiment of the present invention is mainly to perform a quality treatment for a material product that needs to form a film, by integrating the deposition step 4 to form a film on the surface of the material to be treated, and then The constant temperature treatment step 2 is used to optimize the film to form a consistent film deposition and material quality process, which is suitable for use in the processing of electronic or semiconductor products.

The first and second preferred embodiments of the method for improving the quality of the low temperature material of the present invention have the following advantages:

(1) Improving the material quality: after the low temperature and high pressure treatment in the constant temperature treatment step 2, the overall uniformity of the grain structure of the material to be treated is higher, and the gap between the crystal grains and the crystal grains is also greatly reduced. In addition, the density and overall coverage of the material can be greatly improved, thereby improving the quality of the material.

(2) Reducing the accumulation of thermal stress: through the constant temperature treatment below 450 °C, compared with the annealing process above 1000 °C in the existing process, the thermal stress inside the low material can be accumulated greatly, and the reliability of the finished product is more It is high and makes the method more suitable for use in the electronics and semiconductor industries where material reliability is critical.

Referring to FIG. 6 , a low-temperature material quality processing device is suitable for performing the above-mentioned low-temperature material quality method for high-quality processing of a material to be processed 100. The low-temperature material quality processing device comprises a body 5 and a processing unit. 6. A deposition unit 7, a delivery unit 8, and a fluid unit 9.

An accommodating space 51 is formed in the body 5 for accommodating the processing equipment required for each program. The processing unit 6 is disposed in the body 5 and located in the accommodating space 51. The processing unit 6 has an available The processing chamber 61 of the material to be processed 100 is accommodated, and the temperature and pressure in the processing chamber 61 are adjustable. In this embodiment, the pressure in the processing chamber 61 can be between 0 and 400 atm. Between the adjustments, and the temperature can be adjusted within a temperature range of 0 to 450 ° C, so that the material to be treated 100 can be exposed to the first supercritical fluid cleaning step as described above while being placed in the processing chamber 61 1. The treatment is carried out under the environmental conditions of the constant temperature treatment step 2 and the second supercritical fluid cleaning step 3.

The deposition unit 7 is disposed in the body 5 and is adjacent to the processing space 6 and adjacent to the processing unit 6. The deposition unit 7 has a deposition chamber 71 for accommodating the material to be processed 100, and can be a film. Plating on the surface of the material to be treated 100. In the present embodiment, the deposition unit 7 is a chemical vapor deposition device, and the detailed structure, configuration and efficacy of the device should be common knowledge in the technical field. The techniques well known to the person are not described here.

The conveying unit 8 is disposed in the body 5 and located in the accommodating space 51, and can carry the material to be processed 100, so that the material to be processed 100 can be processed in the processing unit 6 and the deposition unit 7 according to a preset process. Access in. In this embodiment, the transport unit 8 can only capture the robot arm of the material to be processed 100, and can put the material to be processed 100 into the processing chamber 61 or the deposition chamber 71 according to a preset flow sequence. It is taken out from the processing chamber 61 or the deposition chamber 71.

The fluid unit 9 is disposed in the body 5 and communicates with the processing chamber 61 of the processing unit 6, and is capable of controlling a fluid 200 to be input into the processing chamber 61. In this embodiment, the fluid unit 9 can Carbon dioxide is introduced into the processing chamber 61 to clean and thermostat the material to be treated 100 in the processing chamber 61, or to extract carbon dioxide from the processing chamber 61 so that the processing chamber 61 is at The state of the vacuum.

In summary, the high-quality treatment of the material to be treated 100 by the constant temperature treatment of low temperature and high pressure can not only enable the processed material to have high density and uniformity, but also avoid heat treatment due to high temperature annealing inside the material. The resulting thermal stress buildup, which in turn enhances the stability of the material, does indeed achieve the objectives of the present invention.

The above is only the preferred embodiment of the present invention, and the scope of the invention is not limited thereto, that is, the simple equivalent changes and modifications made by the scope of the invention and the description of the invention are All remain within the scope of the invention patent.

1. . . First supercritical fluid cleaning step

2. . . Constant temperature processing step

3. . . Second supercritical fluid cleaning step

4. . . Deposition step

5. . . Ontology

51. . . Housing space

6. . . Processing unit

61. . . Processing chamber

7. . . Deposition unit

71. . . Deposition chamber

8. . . Conveyor unit

9. . . Fluid unit

100. . . Material to be treated

200. . . fluid

1 is a flow chart showing a first preferred embodiment of the method for improving the quality of a low temperature material of the present invention;

Figure 2 is a microscopic photomicrograph to assist in explaining the first preferred embodiment;

Figure 3 is a microscopic perspective view of the first preferred embodiment;

Figure 4 is a microscopic photomicrograph to assist in explaining the first preferred embodiment;

Figure 5 is a flow chart showing a second preferred embodiment of the method for improving the quality of the low temperature material of the present invention;

Fig. 6 is a schematic view showing the arrangement of a device for explaining a high-quality processing apparatus for a low temperature material of the present invention.

1. . . First supercritical fluid cleaning step

2. . . Constant temperature processing step

3. . . Second supercritical fluid cleaning step

Claims (7)

A method for improving the quality of a low-temperature material comprises: a first supercritical fluid cleaning step of first placing a material to be treated in a vacuum environment, and then cleaning the material to be treated with a fluid in a supercritical state; a processing step of exposing the material to be treated after the first supercritical fluid cleaning step to a pressure of 70 to 400 atmospheres and a temperature of 100 to 450 degrees Celsius; and a second supercritical fluid cleaning step. The material to be treated that has passed through the thermostatic treatment step is cleaned with a fluid in a supercritical state. According to the method of claim 1, wherein in the constant temperature treatment step, the material to be treated after being cleaned by the first supercritical fluid cleaning step is exposed to a pressure of 200 atm and a temperature. In a vacuum environment of 180 degrees Celsius. The method for improving the quality of a low temperature material according to the first aspect of the invention, wherein the pressure and temperature are changed with time in the constant temperature treatment step. The method for improving the quality of the low temperature material according to any one of claims 1 to 3, further comprising a deposition step between the first supercritical fluid cleaning step and the constant temperature treatment step, wherein the deposition step is The surface of the material to be treated which has been cleaned by the first supercritical fluid cleaning step forms a film. According to the method of claim 4, wherein in the first supercritical fluid cleaning step and the second supercritical fluid cleaning step, the fluid is selected from the group consisting of carbon dioxide and nitrous oxide. Trifluorochloromethane, difluoromethylene chloride or a combination of these. The method for improving the quality of a low temperature material according to claim 5, wherein in the depositing step, the method is selected from the group consisting of sputtering, sintering, physical vapor deposition, arc physical vapor deposition, chemical vapor deposition, or The film is deposited on the surface of the material to be treated by means of electron cyclotron resonance chemical vapor deposition. The invention relates to a high-quality processing device for a low-temperature material, which comprises: a body having a receiving space formed therein; a processing unit disposed on the body and located in the receiving space of the body; The processing unit has a processing chamber, and the temperature and pressure in the processing chamber are adjustable; a deposition unit is disposed in the body and located in the housing space of the body, the deposition unit has a deposition chamber And a film can be plated on the surface of the material to be processed; a conveying unit is disposed on the body and located in the accommodating space of the body and carries the material to be processed, so that the processing unit is processed according to a preset process And accessing the deposition unit; and a fluid unit disposed in the body and in communication with the processing chamber of the processing unit and capable of controlling a fluid to be input into the processing chamber.