JP2012246516A - Method for manufacturing film formed body by vapor deposition - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a method for manufacturing a film formed body by vapor deposition, by which an accuracy of a film thickness of a vapor deposition film is improved.SOLUTION: A vapor deposition apparatus and a member to be subjected to vapor deposition are prepared. The vapor deposition apparatus includes a vacuum chamber and a vapor deposition source. The vapor deposition source is installed within the vacuum chamber and evaporates a deposition material. After the vapor deposition apparatus and the member to be subjected to vapor deposition have been prepared, the member to be subjected to vapor deposition is housed within the vacuum chamber. After the member to be subjected to vapor deposition has been housed within the vacuum chamber, evacuation from an inside of the vacuum chamber is started and the inside of the vacuum chamber is made into a reduced pressure state. After the inside of the vacuum chamber has been made into the reduced pressure state, evaporation of the deposition material from the vapor deposition source is started and a vapor deposition film composed of the deposition material is formed on the member to be subjected to vapor deposition. After the evaporation of the deposition material from the vapor deposition source has been started, evaporation of the deposition material from the vapor deposition source is terminated. At the same time, the evacuation from the inside of the vacuum chamber is terminated and gas is introduced into the inside of the vacuum chamber to release the reduced pressure state.

Description

  The present invention relates to a method for producing a deposited film forming body.

  When the deposition material is deposited on the deposition object such as a substrate by the deposition method, the deposition object is held in a holder installed in the vacuum chamber, the vacuum chamber is depressurized, and the deposition is installed in the vacuum chamber. The vapor deposition material is evaporated from the source. The evaporated deposition material adheres to the deposition target, and a deposition film made of the deposition material is formed on the deposition target. After the deposited film is formed, the vacuum chamber is opened to the atmosphere, and the deposition object on which the deposited film is formed is recovered from the vacuum chamber. In order to make the thickness of the deposited film uniform, the holder is rotated.

  Generally, after the deposited film is formed, the vacuum chamber is maintained in a reduced pressure state for at least 10 minutes. This is to prevent deterioration of the vapor deposition source and discharge the vapor deposition material floating in the vacuum chamber from the vacuum chamber.

  In general, when the vacuum chamber is opened to the atmosphere, the rotation of the holder is stopped. This is to prevent deterioration of the equipment and improve work safety.

  Furthermore, generally, as the name suggests, the atmosphere is released by introducing the atmosphere into the vacuum chamber.

  For example, Patent Document 1 describes that the rotation of the holder is stopped after the gold film is formed, and the vacuum chamber is opened to the atmosphere after the gold film is formed and the temperature is lowered (paragraph 0024, FIG. 2 and FIG. 3).

JP 2011-74442 A

  When a vapor deposition film having a film thickness of several tens of nm is formed by a general vapor deposition method, the variation in film thickness may exceed several nm. For example, in a general vapor deposition method, the actual film thickness may deviate by about ± 5% from the target film thickness. When the target film thickness is 40 to 50 nm, the actual film thickness is the target film thickness. May deviate by about ± 2 to 5 nm. However, there are applications where variations in film thickness exceeding several nm are undesirable. For example, in a metal film that is in close contact with a reflecting surface of a prism provided in an inspection chip used for measurement by surface plasmon resonance (SPR) or surface plasmon excitation fluorescence spectroscopy (SPFS), the film thickness varies by several nm. Affects measurement accuracy.

  The present invention is made to solve this problem. The objective of this invention is providing the manufacturing method of the vapor deposition film forming body which the precision of the film thickness of a vapor deposition film improves.

  The first to fifth aspects of the present invention are directed to a method for producing a deposited film forming body.

  In the first aspect of the present invention, a vapor deposition apparatus and a deposition target are prepared. The vapor deposition apparatus includes a vacuum chamber and a vapor deposition source. A vapor deposition source is installed in a vacuum chamber and evaporates vapor deposition material.

  After the deposition apparatus and the deposition object are prepared, the deposition object is accommodated in the vacuum chamber.

  After the deposition object is accommodated in the vacuum chamber, evacuation from the vacuum chamber is started, and the vacuum chamber is decompressed.

  After the vacuum chamber is depressurized, evaporation of the vapor deposition material from the vapor deposition source is started, and a vapor deposition film made of the vapor deposition material is formed on the deposition target.

  After evaporation of the deposition material from the deposition source is started, evaporation of the deposition material from the deposition source is terminated. At the same time, exhaust from the vacuum chamber is terminated, gas is introduced into the vacuum chamber, and the reduced pressure state is eliminated.

  The second aspect of the present invention adds further matters to the first aspect of the present invention. In the second aspect of the present invention, the vapor deposition apparatus further includes a holder. The holder is installed in the vacuum chamber and holds the deposition target. The rotation of the holder is started before the evaporation of the evaporation material from the evaporation source is started. After the gas is introduced into the vacuum chamber and the reduced pressure state is eliminated, the rotation of the holder is terminated.

  The third aspect of the present invention adds further matters to the second aspect of the present invention. In the third aspect of the present invention, the holder is rotated at a rotation speed of 50 rotations / minute or more and 250 rotations / minute or less.

  The fourth aspect of the present invention adds a further matter to any one of the first to third aspects of the present invention. In the fourth aspect of the present invention, the gas is nitrogen gas or argon gas having a purity of 99.9% or more.

  Preferably, the vapor deposition material is gold.

  According to the first aspect of the present invention, at the same time as the evaporation of the vapor deposition material is completed, the mean free path of the vapor deposition material is abruptly shortened, and the vapor deposition material floating in the vacuum chamber does not reach the deposition object. . Thereby, the increase in the film thickness of the vapor deposition film after the evaporation of the vapor deposition material is suppressed, and the accuracy of the film thickness of the vapor deposition film is improved.

  According to the second aspect of the present invention, the timing of gas contact with the vapor deposition film forming body becomes uniform, the film thickness of the vapor deposition film becomes more uniform, and the accuracy of the film thickness of the vapor deposition film is further improved.

  According to the third aspect of the present invention, the film thickness of the vapor deposition film becomes more uniform, and the accuracy of the film thickness of the vapor deposition film is further improved.

  According to the fourth aspect of the present invention, the deposited film is unlikely to deteriorate. In addition, the deposited film is less likely to become unstable. Furthermore, the film thickness of the deposited film is less affected by atmospheric conditions, and the film thickness accuracy of the deposited film is further improved.

  These and other objects, features, aspects and advantages of the invention will become more apparent from the following detailed description of the invention when considered in conjunction with the accompanying drawings.

It is a schematic diagram which shows the outline of an idea. It is a schematic diagram which shows the outline of an idea. It is a schematic diagram which shows desirable embodiment of a vapor deposition apparatus. It is a flowchart which shows the procedure of vapor deposition. It is sectional drawing of a test | inspection chip. It is a disassembled perspective view of a test | inspection chip. It is a schematic diagram which shows the vicinity of a flow path. It is a schematic diagram which shows the vicinity of a flow path. It is a graph which shows the relationship between the film thickness of a gold film, and an electric field enhancement intensity.

(Outline of the idea)
1 and 2 schematically show the idea.

  When a vapor deposition film is formed by the vapor deposition method, as shown in FIG. 1, the gas is exhausted from the vacuum chamber 100, and the vacuum chamber 100 is decompressed. Thereby, the gas molecule 190 in the vacuum chamber 100 decreases, and the mean free path of the vapor deposition material 192 becomes longer. In this state, evaporation of the vapor deposition material 192 from the vapor deposition source 102 is started. The deposition material 192 scatters from the deposition source 102 to the deposition target 194, the deposition material 192 adheres to the deposition target 194, and a deposition film 196 made of the deposition material 192 is formed on the deposition target 194.

  As shown in FIG. 2, when the film thickness of the vapor deposition film 196 reaches the target and the target vapor deposition film forming body 198 is obtained, the evaporation of the vapor deposition material 192 from the vapor deposition source 102 is terminated. At the same time, exhaust from the vacuum chamber 100 is terminated, gas is introduced into the vacuum chamber 100, and the reduced pressure state is eliminated. Thereby, the gas molecules 190 in the vacuum chamber 100 increase, and the mean free path of the vapor deposition material 192 is abruptly shortened. When the mean free path of the vapor deposition material 192 is shortened, the vapor deposition material 192 floating in the vacuum chamber 100 does not reach the deposition target 194. This contributes to suppressing the increase in the thickness of the vapor deposition film 196 after the evaporation of the vapor deposition material 192 from the vapor deposition source 102 is finished, and improving the accuracy of the film thickness of the vapor deposition film 196.

  The “evaporation method” refers to a film formation method in which a vapor deposition material is evaporated, the evaporation material is advanced from a vapor deposition source to a deposition target through a space, and the deposition material is attached to the deposition target. The method for evaporating the vapor deposition material is not limited. The “deposition method” includes sputtering as well as resistance heating evaporation and electron beam evaporation. The “gas molecule” may be either a monoatomic molecule or a polyatomic molecule.

(Vapor deposition equipment)
The schematic diagram of FIG. 3 shows a preferred embodiment of the vapor deposition apparatus.

  As shown in FIG. 3, the vapor deposition apparatus 1000 includes a vacuum chamber 1002, a vapor deposition source 1004, a substrate holder 1006, a substrate holder rotating mechanism 1008, a shutter 1010, a shutter opening / closing mechanism 1012, a main valve 1014, an exhaust pump 1016, and an atmospheric pressure opening valve. 1018, a gas supply source 1020, a crystal oscillator thickness meter 1022, a controller 1024, an exhaust path 1036, and an intake path 1038. The quartz oscillator thickness meter 1022 includes a sensor 1030 and a main body 1032. The vapor deposition apparatus 1000 is suitably used for forming a gold film having a film thickness of 100 nm or less. However, the vapor deposition apparatus 1000 may be used to form a film having a thickness greater than 100 nm, or the vapor deposition apparatus 1000 may be used to form a vapor deposition film other than a gold film.

  The form of the vapor deposition source 1004 is not limited. The vapor deposition source 1004 is, for example, a plasma assisted sputtering gun, an electron gun, an RF (high frequency) magnetron cathode, a resistance heating evaporation source, or the like. The vapor deposition source 1004 is installed in the vacuum chamber 1002. While the vapor deposition source 1004 is functioning, the vapor deposition material evaporates from the vapor deposition source 1004.

  The substrate holder 1006 is installed in the vacuum chamber 1002. The substrate holder 1006 holds the substrate 1900.

  The substrate 1900 is a deposition object on which a gold film is formed. The deposition object may have a shape that is difficult to call a “substrate”. For example, the deposition object may be a rod, a tube, a block, a film, or the like.

  The substrate holder rotation mechanism 1008 rotates the substrate holder 1006 around the rotation axis 1034. The rotating shaft 1034 extends in a direction from the vapor deposition source 1004 toward the substrate holder 1006.

  The shutter 1010 inhibits the evaporation material from scattering.

  The shutter opening / closing mechanism 1012 opens and closes the shutter 1010. When the shutter 1010 is opened, the shutter 1010 is retracted from between the vapor deposition source 1004 and the substrate holder 1006. When the shutter 1010 is closed, the shutter 1010 is inserted between the vapor deposition source 1004 and the substrate holder 1006.

  The main valve 1014 opens and closes an exhaust path 1036 from the vacuum chamber 1002. When the main valve 1014 is closed, gas is not exhausted from the vacuum chamber 1002. When the main valve 1014 is opened, gas is exhausted from the vacuum chamber 1002. When the main valve 1014 is opened while the atmospheric pressure release valve 1018 is closed, the inside of the vacuum chamber 1002 is decompressed. The reduced pressure state is desirably 0.001 times or less of atmospheric pressure, and more desirably 0.0001 times or less of atmospheric pressure.

  The exhaust pump 1016 is connected to the exhaust path 1036 and exhausts gas from the vacuum chamber 1002 via the main valve 1014. The exhaust pump 1016 is a combination of a rotary pump and a diffusion pump, a turbo molecular pump, or the like.

  The atmospheric pressure release valve 1018 opens and closes the intake path 1038 into the vacuum chamber 1002. When the atmospheric pressure release valve 1018 is closed, no gas is supplied into the vacuum chamber 1002. When the atmospheric pressure release valve 1018 is opened, gas is supplied into the vacuum chamber 1002. When the atmospheric pressure release valve 1018 is opened while the main valve 1014 is closed, the reduced pressure state in the vacuum chamber 1002 is eliminated.

  The gas supply source 1020 is connected to the intake path 1038 and supplies gas into the vacuum chamber 1002 via the atmospheric pressure release valve 1018. The gas supply source 1020 is a cylinder, factory piping, or the like.

  The sensor 1030 includes a crystal resonator. The sensor 1030 is disposed near the substrate 1900. The main body 1032 is installed outside the vacuum chamber 1002. The main body 1032 obtains the thickness of the vapor deposition film from the decrease in the resonance frequency of the crystal resonator due to the vapor deposition film attached to the crystal resonator.

  The controller 1024 controls the vapor deposition source 1004, the substrate holder rotation mechanism 1008, the shutter opening / closing mechanism 1012, the main valve 1014, and the atmospheric pressure release valve 1018, and acquires the film thickness measurement result from the quartz oscillator film thickness meter 1022. The controller 1024 is a computer in which a program is installed. All or part of the functions of the controller 1024 may be carried by hardware without a program. The hardware is, for example, an electronic circuit including an operational amplifier and a comparator.

(Deposition procedure)
The flowchart of FIG. 4 shows the procedure of vapor deposition using a vapor deposition apparatus.

  In vapor deposition, a vapor deposition apparatus 1000 is prepared (step S101), and a substrate 1900 is prepared (step S102).

  After the vapor deposition apparatus 1000 and the substrate 1900 are prepared, the substrate 1900 is held by the substrate holder 1006 (step S103). Thereby, the substrate 1900 is accommodated in the vacuum chamber 1002.

  After the substrate 1900 is accommodated in the vacuum chamber 1002, the main valve 1014 is opened (step S104). Thereby, the exhaust from the inside of the vacuum chamber 1002 is started, and the inside of the vacuum chamber 1002 is brought into a reduced pressure state. At this time, the atmospheric pressure release valve 1018 remains closed.

  After the vacuum chamber 1002 is depressurized, the substrate holder rotating mechanism 1008 starts to rotate the substrate holder 1006 (step S105).

  After the vacuum chamber 1002 is depressurized and the rotation of the substrate holder 1006 is started, the shutter opening / closing mechanism 1012 opens the shutter 1010, the deposition source 1004 is functioned, and evaporation of the deposition material from the deposition source 1004 starts. (Step S106). Thereby, a vapor deposition film is formed on the substrate 1900.

  After evaporation of the vapor deposition material from the vapor deposition source 1004 is started, the thickness of the vapor deposition film is monitored by the crystal oscillator film thickness meter 1022. When the film thickness of the vapor deposition film does not reach the target, evaporation of the vapor deposition material from the vapor deposition source 1004 is continued ("NO" in step S107). When the film thickness of the vapor deposition film reaches the target (“YES” in step S107), the shutter opening / closing mechanism 1012 closes the shutter 1010, the function of the vapor deposition source 1004 is stopped, and vapor deposition material from the vapor deposition source 1004 is evaporated. The process is terminated (step S108).

  At the same time as the evaporation of the vapor deposition material from the vapor deposition source 1004 is terminated, the main valve 1014 is closed (step S109). Thereby, exhaust from the vacuum chamber 1002 is completed.

  At the same time as the evaporation of the vapor deposition material from the vapor deposition source 1004 is terminated, the atmospheric pressure release valve 1018 is opened (step S110). As a result, gas is introduced into the vacuum chamber 1002, the reduced pressure state in the vacuum chamber 1002 is eliminated, and the vacuum chamber 1002 is opened to atmospheric pressure.

  When gas is introduced into the vacuum chamber 1002, the inside of the vacuum chamber 1002 returns to atmospheric pressure. However, the pressure in the vacuum chamber 1002 after the gas is introduced into the vacuum chamber 1002 may be slightly different from the atmospheric pressure, for example, 0.8 times to 1.2 times the atmospheric pressure.

  Since the evaporation source 1004 is sufficiently water-cooled, there is no problem even if the vacuum chamber 1002 is opened to the atmospheric pressure at the same time as the evaporation of the evaporation material from the evaporation source 1004 is completed. Further, in the case where the vapor deposition material is gold, there is no influence on the environment even if the vapor deposition material (gold) floating in the vacuum chamber 1002 due to the release of atmospheric pressure diffuses into the atmosphere.

  The gas supplied into the vacuum chamber 1002 is desirably nitrogen gas or argon gas having a purity of 99.9% or more. Thereby, even if the pressure in the vacuum chamber 1002 changes rapidly, a vapor deposition film does not deteriorate easily. Further, even if the pressure in the vacuum chamber 1002 changes suddenly, the deposited film is unlikely to become unstable. Furthermore, the film thickness of the deposited film is less susceptible to atmospheric conditions, and the film thickness accuracy of the deposited film is improved. There is a problem that it is rare, but the gas may be helium gas. Although there is a problem that management is difficult because the composition is not constant, the gas may be sufficiently dry air.

  After the gas is introduced into the vacuum chamber 1002 and the inside of the vacuum chamber 1002 returns to atmospheric pressure, the substrate holder rotating mechanism 1008 ends the rotation of the substrate holder 1006 (step S111). As a result, the substrate holder 1006 is rotated when the gas is introduced into the vacuum chamber 1002, and the timing of the gas contact with the substrate 1900 on which the vapor deposition film is formed becomes uniform. The film thickness accuracy is further improved. On the contrary, when the substrate holder 1006 is not rotated when the gas is introduced into the vacuum chamber 1002, the timing of the gas contact with the substrate 1900 on which the vapor deposition film is formed becomes uneven, and the vapor deposition film The film thickness becomes non-uniform. This is because when the gas contacts the substrate 1900 on which the vapor deposition film is formed, the film thickness of the vapor deposition film increases. However, even when the substrate holder 1006 is not rotated when the gas is introduced into the vacuum chamber 1002, the above-described idea is not completely lost.

  The number of rotations of the substrate holder 1006 is desirably 50 rotations / minute or more and 250 rotations / minute or less. This is because if the rotation number of the substrate holder 1006 is within this range, the film thickness of the vapor deposition film becomes uniform, and the accuracy of the film thickness of the vapor deposition film is further improved. When the rotation speed of the substrate holder 1006 is slower than this range, the effect of making the gas contact timing uniform to the substrate 1900 on which the vapor deposition film is formed is less likely to appear, and the film thickness of the vapor deposition film tends to be non-uniform. Because. This is because when the rotation number of the substrate holder 1006 is faster than this range, the rotation of the substrate holder 1006 generates convection, and the film thickness variation of the deposited film tends to increase. In many cases, the substrate holder rotating mechanism 1008 is designed on the assumption that it is operated when the inside of the vacuum chamber 1002 is in a reduced pressure state. The substrate holder rotating mechanism 1008 is likely to deteriorate.

  The above-described vapor deposition procedure may be automatically executed by the controller 1024 or may be manually executed by an operator. Automatic execution by the controller 1024 and manual work by an operator may be mixed.

(Use)
Although the use of the above-described vapor deposition method is not limited, it is desirable to form a gold film on the reflecting surface of the prism of an inspection chip used for measurement by surface plasmon resonance (SPR) or surface plasmon excitation fluorescence spectroscopy (SPFS). The above vapor deposition method is used.

  The schematic diagrams of FIGS. 5 and 6 show a preferred embodiment of the test chip. FIG. 5 is a cross-sectional view. FIG. 6 is an exploded perspective view.

  As shown in FIGS. 5 and 6, the inspection chip 1100 includes a prism 1150, a gold film 1152, a carboxymethyl dextran (CMD) film 1154, a flow path member 1156, a lid member 1158, and a seal member 1160. Other components may be added to the inspection chip 1100. The inspection chip 1100 is also called a sensor chip, an analysis chip, a sample cell, or the like. A channel 1162 is formed in the channel member 1156. Through holes 1164 and 1166 are formed in the lid member 1158.

  7 and 8 show the vicinity of the flow path.

  When measurement is performed using the test chip 1100, as shown in FIG. 7, the sample liquid 1202 is supplied to the flow path 1162, and the antigen 1058 contained in the sample liquid 1202 and the antibody 1064 immobilized on the CMD film 1154 Is reacted.

  Subsequently, as shown in FIG. 8, a labeled antibody solution 1196 is supplied to the flow path 1162, and the antigen 1058 and the labeled antibody 1062 are reacted.

  Subsequently, the excitation light is applied to the prism 1150. The excitation light is reflected at the interface between the prism 1150 and the gold film 1152. When excitation light is reflected at the interface between the prism 1150 and the gold film 1152, the evanescent wave 1082 leaks from the interface between the gold film 1152 and the prism 1150 toward the gold film 1152, and plasmons on the surface of the gold film 1152. And the evanescent wave 1082 interfere with each other. When the plasmon and the evanescent wave 1082 resonate, the electric field of the evanescent wave 1082 is significantly enhanced. As shown in FIG. 8, the enhanced electric field excites the labeled antibody 1062, and surface plasmon excitation fluorescence 1044 is emitted from the labeled antibody 1062.

  The graph of FIG. 9 shows the relationship between the thickness of the gold film for each material composing the prism 1050 and the electric field enhancement with respect to excitation light having a wavelength of 635 nm. Table 1 shows the physical properties of the material constituting the prism.

  As shown in FIG. 9 and Table 1, when the refractive index of the material is high, the change in the electric field enhancement due to the film thickness becomes large, and strict film thickness management is required. When the refractive index of the material is low, the change in the electric field enhancement intensity due to the film thickness is small, but the optimum film thickness at which the electric field enhancement intensity is maximized becomes thin, so that strict film thickness management is still required. Further, when the CMD film 1154 is fixed on the surface of the gold film 1152, the sensitivity difference is further increased. That is, strict film thickness control is required regardless of the refractive index of the resin material.

Example 1
A gold film was formed on the substrate 1900 made of glass SLAL10 by a sputtering method using a plasma-assisted sputtering gun as the vapor deposition source 1004 according to the above vapor deposition procedure. The target thickness of the gold film was 44 nm. The main body 1032 was set so that the indicated value of the crystal oscillator thickness meter 1022 was 10 times the actual film thickness.

The formation of the gold film was completed at the same time as the reading of the crystal oscillator thickness meter 1022 showed 440. Simultaneously with completion, the function of the plasma assisted sputtering gun was stopped, the main valve 1014 was closed, and the atmospheric pressure release valve 1018 was opened. Nitrogen gas having a purity of 99.9% was introduced into the vacuum chamber 1002 at a pressure of 1 kgf / cm ² . The rotation of the substrate holder 1006 was continued until the inside of the vacuum chamber 1002 returned to atmospheric pressure. The rotation speed of the substrate holder 1006 was 220 rotations / minute.

  The thickness of the gold film was observed with a focused ion beam-transmission electron microscope (FIB-TEM). The film thickness of the gold film can also be obtained by calculation from the refractive index n and extinction coefficient k of the gold film measured with a spectroscope.

  In the first trial, the film thickness of the gold film formed on the 16 substrates 1900 was 44 to 45 nm.

  Even in the second trial, the film thickness of the gold film formed on the 16 substrates 1900 was 44 to 45 nm.

(Comparative Example 1)
A gold film is formed in the same manner as in Example 1 except that the main valve 1014 is closed after 30 minutes from the stop of the function of the plasma-assisted sputtering gun, and then the atmospheric pressure release valve 1018 is opened. Formed.

  In the first trial, the film thickness of the gold film formed on 16 substrates 1900 was 46 to 47 nm.

  In the second trial, the film thickness of the gold film formed on the 16 substrates 1900 was 45 to 46 nm.

(Comparison between Example 1 and Comparative Example 1)
When Example 1 is compared with Comparative Example 1, it can be seen that in Example 1, the actual film thickness approaches the target, the reproducibility of the film thickness is improved, and the film thickness accuracy can be improved.

(Example 2)
A gold film was formed on the substrate 1900 made of resin E48R (cycloolefin polymer resin manufactured by Nippon Zeon Co., Ltd.) using an electron gun as the vapor deposition source 1004 according to the above vapor deposition procedure. The target for the thickness of the gold film was 38 nm. The main body 1032 was set so that the indicated value of the crystal oscillator thickness meter 1022 was 10 times the actual film thickness.

The formation of the gold film was completed at the same time as the reading of the crystal oscillator thickness meter 1022 indicated 380. Simultaneously with the completion, the function of the electron gun was stopped, the main valve 1014 was closed, and the atmospheric pressure release valve 1018 was opened. Argon gas having a purity of 99.9% was introduced into the vacuum chamber 1002 at a pressure of 1 kgf / cm ² . The rotation of the substrate holder 1006 was continued until the inside of the vacuum chamber 1002 returned to atmospheric pressure. The rotation speed of the substrate holder 1006 was 50 rotations / minute.

  The thickness of the gold film was observed by FIB-TEM.

  In the first trial, the film thickness of the gold film formed on 16 substrates 1900 was 38 to 39 nm.

  Even in the second trial, the film thickness of the gold film formed on the 16 substrates 1900 was 38 to 39 nm.

(Comparative Example 2)
Except that the main valve 1014 is closed after 30 minutes have passed since the electron gun function was stopped, the atmospheric pressure release valve 1018 is opened, and the rotation of the substrate holder 1006 is terminated when the main valve 1014 is closed. In the same manner as in Example 2, a gold film was formed.

  In the first trial, the film thickness of the gold film formed on the 16 substrates 1900 was 40 to 45 nm.

  In the second trial, the film thickness of the gold film formed on the 16 substrates 1900 was 42 to 46 nm.

(Comparison between Example 2 and Comparative Example 2)
When Example 2 is compared with Comparative Example 2, in Example 2, the actual film thickness approaches the target, the film thickness variation is reduced, the film thickness reproducibility is improved, and the film thickness accuracy can be improved. I understand. Continuing the rotation of the substrate holder 1006 until the inside of the vacuum chamber 1002 returns to the atmospheric pressure contributes to reducing variations in the batch.

(Example 3)
A gold film was formed on the substrate 1900 made of glass BK7 by a sputtering method using an RF magnetron cathode as the vapor deposition source 1004 according to the above vapor deposition procedure. The target of the gold film thickness was 41 nm. The main body 1032 was set so that the indicated value of the crystal oscillator thickness meter 1022 was 10 times the actual film thickness.

The formation of the gold film was completed at the same time that the reading of the crystal oscillator thickness meter 1022 showed 410. Simultaneously with completion, the function of the RF magnetron cathode was stopped, the main valve 1014 was closed, and the atmospheric pressure release valve 1018 was opened. Nitrogen gas having a purity of 99.9% was introduced into the vacuum chamber 1002 at a pressure of 1 kgf / cm ² . The rotation of the substrate holder 1006 was continued until the inside of the vacuum chamber 1002 returned to atmospheric pressure. The rotation speed of the substrate holder 1006 was 130 rotations / minute.

  The thickness of the gold film was observed by FIB-TEM.

  In the first trial, the film thickness of the gold film formed on the 16 substrates 1900 was 41 to 42 nm.

  Even in the second trial, the film thickness of the gold film formed on the 16 substrates 1900 was 41 to 42 nm.

(Comparative Example 3)
After 30 minutes have passed since the function of the RF magnetron cathode is stopped, the main valve 1014 is closed, then the atmospheric pressure release valve 1018 is opened, the surrounding air is introduced into the vacuum chamber 1002, and the main valve 1014 is closed. A gold film was formed in the same manner as in Example 3 except that the rotation of the substrate holder 1006 was occasionally completed. The film thickness of the gold film formed on 16 substrates 1900 was 43 to 48 nm.

  When comparing rainy days and clear days, the film thicknesses of the gold films formed on the 16 substrates 1900 were 47 to 51 nm and 43 to 47 nm, respectively.

(Comparison between Example 3 and Comparative Example 3)
When Example 3 is compared with Comparative Example 3, in Example 3, the actual film thickness approaches the target, the film thickness variation is reduced, the film thickness reproducibility is improved, and the film thickness accuracy can be improved. I understand. It can also be seen that it is not easily affected by the weather.

  While the invention has been shown and described in detail, the above description is illustrative in all aspects and not restrictive. Accordingly, it is understood that numerous modifications and variations can be devised without departing from the scope of the present invention.

1000 Vapor deposition apparatus 1002 Vacuum tank 1004 Vapor deposition source 1006 Substrate holder 1014 Main valve 1018 Atmospheric pressure release valve 1900 Substrate

Claims (5)

A method for producing a deposited film forming body, comprising:
(a) preparing a vapor deposition apparatus including a vacuum chamber and a vapor deposition source installed in the vacuum chamber to evaporate a vapor deposition material;
(b) a step of preparing a deposition object;
(c) after the step (a) and the step (b), the step of accommodating the deposition object in the vacuum chamber;
(d) after the step (c), starting the exhaust from the vacuum chamber, and making the vacuum chamber in a reduced pressure state;
(e) after the step (d), starting evaporation of the vapor deposition material from the vapor deposition source, and forming a vapor deposition film made of the vapor deposition material on the deposition object;
(f) after the step (e), terminating the evaporation of the vapor deposition material from the vapor deposition source;
(g) simultaneously with the step (f), ending the exhaust from the vacuum chamber;
(h) simultaneously with the step (f), introducing a gas into the vacuum chamber, and eliminating the reduced pressure state;
The manufacturing method of a vapor deposition film forming body provided with. In the manufacturing method of the vapor deposition film forming body of Claim 1,
The vapor deposition apparatus further includes a holder that is installed in the vacuum chamber and holds the deposition object,
In the step (c), the deposition object is held in the holder,
The method for producing the deposited film forming body is
(i) starting rotation of the holder before the step (e);
(j) ending rotation of the holder after step (h);
The manufacturing method of the vapor deposition film forming body further equipped with these. In the manufacturing method of the vapor deposition film forming body of Claim 2,
The manufacturing method of the vapor deposition film formation body which rotates the said holder by the rotation speed of 50 rotation / min or more and 250 rotation / min or less. In the manufacturing method of the vapor deposition film forming body in any one of Claim 1- Claim 3,
The said gas is a manufacturing method of the vapor deposition film forming body whose purity is 99.9% or more of nitrogen gas or argon gas. In the manufacturing method of the vapor deposition film forming body in any one of Claim 1- Claim 4,
The manufacturing method of the vapor deposition film formation body whose said vapor deposition material is gold | metal | money.

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