CN117888061A - Silver metal evaporation vacuum coating method - Google Patents
Silver metal evaporation vacuum coating method Download PDFInfo
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- CN117888061A CN117888061A CN202410289062.2A CN202410289062A CN117888061A CN 117888061 A CN117888061 A CN 117888061A CN 202410289062 A CN202410289062 A CN 202410289062A CN 117888061 A CN117888061 A CN 117888061A
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- 238000000034 method Methods 0.000 title claims abstract description 56
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 238000001771 vacuum deposition Methods 0.000 title claims abstract description 27
- 238000001883 metal evaporation Methods 0.000 title claims abstract description 9
- 238000001704 evaporation Methods 0.000 claims abstract description 152
- 230000008020 evaporation Effects 0.000 claims abstract description 134
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims abstract description 61
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 60
- 239000011733 molybdenum Substances 0.000 claims abstract description 60
- 229910052751 metal Inorganic materials 0.000 claims abstract description 41
- 239000002184 metal Substances 0.000 claims abstract description 41
- 238000002844 melting Methods 0.000 claims abstract description 40
- 230000008018 melting Effects 0.000 claims abstract description 40
- 239000007769 metal material Substances 0.000 claims abstract description 21
- 229910052709 silver Inorganic materials 0.000 claims abstract description 14
- 239000004332 silver Substances 0.000 claims abstract description 14
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 31
- 229910052802 copper Inorganic materials 0.000 claims description 31
- 239000010949 copper Substances 0.000 claims description 31
- 239000000463 material Substances 0.000 claims description 16
- 238000000576 coating method Methods 0.000 claims description 11
- 239000011248 coating agent Substances 0.000 claims description 8
- 239000000758 substrate Substances 0.000 claims description 7
- 238000007747 plating Methods 0.000 claims description 5
- 238000004544 sputter deposition Methods 0.000 abstract description 24
- 239000012535 impurity Substances 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 239000007888 film coating Substances 0.000 abstract description 3
- 238000009501 film coating Methods 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 32
- 235000012431 wafers Nutrition 0.000 description 16
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 5
- 229910052721 tungsten Inorganic materials 0.000 description 5
- 239000010937 tungsten Substances 0.000 description 5
- 238000001816 cooling Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000010894 electron beam technology Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 239000007770 graphite material Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000002932 luster Substances 0.000 description 2
- 238000010309 melting process Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 230000000087 stabilizing effect Effects 0.000 description 2
- 241000120551 Heliconiinae Species 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention discloses a silver metal evaporation vacuum coating method, and relates to the technical field of vacuum coating. By placing a molybdenum crucible in a crucible of an evaporation device, and taking the molybdenum crucible as a container for evaporating a film coating of a silver metal material, the melting point of silver is far less than that of molybdenum, and the melting source process can not lead to melting or deformation of the molybdenum crucible; the heat is not easy to dissipate after the molybdenum crucible is added, the power of a melting source is reduced, metal is completely melted in the molybdenum crucible, a metal material is in close contact with the molybdenum crucible, air and impurities are not contained in the metal, and the frequency of a metal source sputtering source in the evaporation process is obviously reduced. The invention divides the process of evaporating vacuum coating into a preheating stage, a premelting stage, an evaporation source melting stage and a stable evaporating stage which are sequentially carried out, and slowly heats up, thereby being beneficial to further avoiding the occurrence of metal source sputtering.
Description
Technical Field
The invention relates to the technical field of vacuum coating, in particular to a silver metal evaporation vacuum coating method.
Background
At present, an evaporation vacuum coating technology is often adopted to form a welding Ag metal film on the surface of a wafer, and in the process, a red copper metal crucible which is provided with evaporation equipment is generally adopted. During the evaporation, the metal is directly put in a red copper crucible for evaporation. The disadvantages of this approach are:
(1) Because the water cooling system is arranged below the red copper crucible, the heat conduction is faster, and the evaporation source material is not easy to melt, so the power required by evaporation is larger. The center of the source material is easily melted in the evaporation process, deformation vacancies appear under the metal after the continuous evaporation for several times, and the metal cannot be in good contact with the red copper crucible.
(2) In addition, the red copper crucible is easy to oxidize at high temperature, and the oxide layer is easy to form a black impurity layer with the metal source material.
Because the Ag metal film has the defects in the preparation process, the film coating needs to be increased in power to melt the metal source material, and because the gas between the deformed metal and the red copper crucible is not easy to be emitted when being heated, the air and the metal source material are not heated uniformly under the condition of continuously heating, the accumulated heat is difficult to be emitted, and the metal sputtering source is easy to be caused. After sputtering, metal points are sputtered on the surface of the light wafer, and the sputtered metal on the heavy wafer is broken, so that serious loss is caused.
In view of this, the present invention has been made.
Disclosure of Invention
The invention aims to provide a silver metal evaporation vacuum coating method, which aims to effectively reduce coating power and avoid the problem of metal source sputtering.
The invention is realized in the following way:
In a first aspect, the present invention provides a method for vapor vacuum coating silver metal, comprising: placing a molybdenum crucible into a crucible of an evaporation device, taking the molybdenum crucible as a container for evaporating and coating silver metal materials, and forming a metal film layer on a substrate by an evaporating vacuum coating method;
The process of evaporating vacuum coating comprises a preheating stage, a premelting stage, an evaporation source melting stage and a stable evaporating stage which are sequentially carried out;
The voltages applied in the preheating stage, the premelting stage, the evaporation source melting stage and the stable evaporation stage are all 9kV-11kV, and the current applied from the preheating stage to the evaporation source melting stage is gradually increased;
In the stable evaporation stage, 48mA-52mA current is firstly applied for 20s-40s, the baffle is opened to start the evaporation process after the evaporation source material is completely melted, the current is reduced to 10mA-20mA, and the evaporation rate of silver metal is controlled to be stabilized at 20A/s-40A/s.
In an alternative embodiment, the applied current is controlled to be 8mA-12mA and the current application time is controlled to be 20s-40s during the preheating stage.
In an alternative embodiment, the applied current is controlled to be 28mA-32mA and the current application time is controlled to be 20s-40s in the premelting stage.
In an alternative embodiment, the current applied is controlled to be 38mA-42mA and the current applied time is controlled to be 20s-40s in the evaporation source melting stage.
In an alternative embodiment, the vacuum is controlled to be (1-3) x 10 -6 torr during evaporation of the vacuum coating.
In an alternative embodiment, the molybdenum crucible has a purity greater than 99.9%, a density of 10.0g/cm 3-10.5g/cm3, and a melting point of 2610 ℃ to 2630 ℃;
preferably, the silver metallic material has a purity of greater than 99.99%, a density of 10.3g/cm 3-10.7g/cm3 and a melting point of 951-971 ℃.
In an alternative embodiment, the crucible of the evaporation apparatus is a red copper crucible.
In an alternative embodiment, the substrate is a wafer.
The invention has the following beneficial effects: by placing a molybdenum crucible in a crucible of an evaporation device, and taking the molybdenum crucible as a container for evaporating a film coating of a silver metal material, the melting point of silver is far less than that of molybdenum, and the melting source process can not lead to melting or deformation of the molybdenum crucible; the heat is not easy to dissipate after the molybdenum crucible is added, the power of a melting source is reduced, metal is completely melted in the molybdenum crucible, a metal material is in close contact with the molybdenum crucible, air and impurities are not contained in the metal, and the frequency of a metal source sputtering source in the evaporation process is obviously reduced. The invention divides the process of evaporating vacuum coating into a preheating stage, a premelting stage, an evaporation source melting stage and a stable evaporating stage which are sequentially carried out, and slowly heats up, thereby being beneficial to further avoiding the occurrence of metal source sputtering.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present invention and should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of a molybdenum crucible according to example 1 of the present invention;
FIG. 2 is a view showing the wafer surface after sputtering source of comparative example 1 and comparative example 2, (a) shows comparative example 1, and (b) shows comparative example 2;
FIG. 3 is a schematic diagram of the plating layers obtained in example 1 and comparative example 4, wherein (a) represents example 1 and (b) represents comparative example 4.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more clear, the technical solutions of the embodiments of the present invention will be clearly and completely described below. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
The embodiment of the invention provides a silver metal evaporation vacuum coating method, which comprises the following steps:
S1, preparation work
A molybdenum crucible, a base material, a silver metal material, and an evaporation apparatus for performing evaporation vacuum plating were prepared, respectively.
Specifically, the molybdenum crucible can be a commercially available component, the purity of molybdenum is more than 99.9% (such as 99.99%), the density is 10.0g/cm 3-10.5g/cm3 (such as about 10.2g/cm 3), and the melting point is 2610-2630 ℃ (such as about 2620 ℃).
Specifically, the type of the substrate is not limited, and may be a commercially available wafer (i.e., silicon wafer), but is not limited thereto.
Specifically, the silver metal material has a purity of greater than 99.99% (e.g., 99.999%) and a density of 10.3g/cm 3-10.7g/cm3 (e.g., about 10.5g/cm 3) and a melting point of 951-971 ℃ (e.g., about 961 ℃). The melting point of molybdenum is far greater than that of silver and is more than 2.5 times that of silver, and the melting source process can not lead to the melting or deformation of the molybdenum crucible.
Specifically, the evaporation apparatus may be a commercially available apparatus, and the model may be EBX2000, but is not limited thereto. In the evaporation apparatus, the crucible is provided, and the metal is generally placed in the crucible to be evaporated. The crucible of the evaporation equipment can be a red copper crucible, and metal is directly placed under the red copper crucible for evaporation in the evaporation process, because a water cooling system is arranged under the red copper crucible, the heat conduction is faster, the evaporation source material is not easy to melt, the evaporation needs high power, the center is easy to melt, and after the continuous evaporation is carried out for several times, the gap appears under the metal, and the metal cannot be well contacted with the red copper crucible; when the power is increased, the metal source is splashed due to uneven heating.
The inventor creatively places the molybdenum crucible in a crucible of the evaporation equipment, takes the molybdenum crucible as a container for evaporating and coating silver metal materials, adopts the molybdenum crucible and the red copper crucible to be combined inaccurately (a gap of 1-2mm is reserved) in the evaporation process, so that heat is not easy to dissipate, and the power of a melting source is reduced; in the evaporation process, after the metal material is fully melted, the metal is in close contact with the molybdenum crucible, so that the problem of source sputtering can be effectively solved, and the frequency of the source sputtering of the metal source in the evaporation process is reduced to zero.
The shape and size of the molybdenum crucible can be as shown in fig. 1, the outer diameter of the bottom wall can be 39±0.25mm, the inner diameter of the bottom wall can be 20±0.25mm, the thickness of the bottom wall is set to 5±0.25mm, the outer diameter of the top can be 44±0.25mm, the inner diameter of the top wall can be 31±0.25mm, and the height can be 24±0.25mm. The inner diameter of the top and the inner diameter of the bottom of the red copper crucible are slightly larger than those of the molybdenum crucible, for example, the inner diameter of the top of the red copper crucible can be 45+/-0.1 mm, the inner diameter of the bottom of the red copper crucible can be 40+/-0.1 mm, and the height of the red copper crucible can be 24+/-0.1 mm. Before coating, the molybdenum crucible is contained in a red copper crucible, a silver metal material is placed in the molybdenum crucible, a baffle plate is covered, and the baffle plate is used for isolating the silver metal material from a substrate (such as a wafer) fixed above.
S2, evaporating vacuum coating
A metal film layer is formed on a substrate by an evaporation vacuum coating method, electrons emitted by an electron beam are incident into the middle of a crucible at a certain angle (270 degrees for example) in the working process, fall into a silver metal material to melt silver metal, the melted metal is gasified along with the increase of evaporation power, and gasified metal atoms fall onto the surface of a wafer in a vacuum chamber to form deposition.
Before evaporating vacuum coating, high vacuum is established, after the high vacuum is established, a power supply is turned on to apply high voltage to an electron gun, an evaporating program is selected, the selected metal crucible is checked to rotate in place, and a current is applied to start melting the source. In some embodiments, the vacuum is controlled to be (1-3) x 10 -6 torr, such as1 x 10 -6torr、2×10-6torr、3×10-6 torr, etc. during evaporation of the vacuum coating.
In some embodiments, the process of evaporating the vacuum coating comprises a preheating stage, a premelting stage, an evaporation source melting stage and a stable evaporation stage which are sequentially carried out, and the process is divided into four stages to operate, and the temperature is slowly increased, so that the occurrence of metal source sputtering is further avoided.
The voltages applied in the preheating stage, the premelting stage, the evaporation source melting stage and the stable evaporation stage are all 9kV-11kV (such as 9kV, 10kV, 11kV and the like), the current applied from the preheating stage to the evaporation source melting stage is gradually increased, in the preheating stage, the applied current is controlled to be 8mA-12mA, and the current application time is controlled to be 20s-40s; in the premelting stage, controlling the applied current to be 28mA-32mA, and controlling the current application time to be 20s-40s; in the evaporation source melting stage, the applied current is controlled to be 38mA-42mA, and the current application time is controlled to be 20s-40s. Specifically, the current applied in the preheating stage can be 8mA, 9mA, 10mA, 11mA, 12mA and the like, and the current application time can be 20s, 25s, 30s, 35s, 40s and the like; the current applied in the premelting stage can be 28mA, 29mA, 30mA, 31mA, 32mA and the like, and the current application time can be 20s, 25s, 30s, 35s, 40s and the like; the current applied in the evaporation source melting stage can be 38mA, 39mA, 40mA, 41mA, 42mA and the like, and the current application time can be 20s, 25s, 30s, 35s, 40s and the like.
The silver metal evaporation rate is controlled to be 20A/s-40A/s in the stable evaporation stage, such as 20A/s, 30A/s, 40A/s, etc. In the actual operation process, 48mA-52mA current is firstly applied in the stable evaporation stage, the application time is 20s-40s, and the evaporation process is started by opening the baffle after the evaporation source material is completely melted. The display screen of the evaporation equipment displays an evaporation rate curve in a stable evaporation stage, after the baffle is opened, the evaporation rate is increased to 50A/s-80A/s because the rate overshoots in a high-power source melting process, and the current is automatically adjusted and reduced to 10mA-20mA along with the equipment setting of the evaporation rate of 30A/s, so that the evaporation rate is stabilized at 20A/s-40A/s. Specifically, the current applied first may be 48mA, 49mA, 50mA, 51mA, 52mA, etc., and the current application time may be 20s, 25s, 30s, 35s, 40s, etc.; opening the baffle starts the evaporation process, and the evaporation rate can be observed to rise to a stable evaporation process, and finally the evaporation rate is stabilized at the set evaporation rate. The thickness of the coating is not more than 5 mu m, and the maximum thickness of different coating of the equipment is also different.
The features and capabilities of the present invention are described in further detail below in connection with the examples.
Example 1
The embodiment provides a silver metal evaporation vacuum coating method, which comprises the following steps:
(1) Preparation work
Preparing a molybdenum crucible: the purity of the molybdenum metal is 99.99%, the density is 10.2g/cm 3, the melting point is about 2620 ℃, and the shape and the size are shown in figure 1.
Preparing a base material: the thickness of the wafer is 450-600mm, and the silicon content is 99.999%.
Preparing a silver metal material: silver particles are commercially available in a purity of 99.99%, a density of 10.5g/cm 3 and a melting point of about 961 ℃.
Preparing an evaporation device: the model of the evaporation vacuum coating equipment is EBX2000, the copper crucible is provided (the inner diameter of the top is 45+/-0.1 mm, the inner diameter of the bottom is 40+/-0.1 mm, and the height is 24+/-0.1), and the copper crucible is positioned below the vacuum chamber and is provided with a water cooling system. Placing the molybdenum crucible in a red copper crucible, placing 60-120g of silver metal material in the molybdenum crucible until the silver metal material is flush with the upper edge of the molybdenum crucible, covering a baffle plate, and isolating the silver metal material and a wafer fixed above the baffle plate.
(2) Evaporation vacuum coating
And (3) establishing high vacuum 2 multiplied by 10 -6 torr by adopting an evaporation vacuum coating technology, and when the high vacuum is established, starting a power supply to apply high voltage to an electron gun to start the electron gun, checking that the molybdenum crucible and the red copper crucible rotate in place, and adding current to start melting the source. The melting source process is divided into four stages, and the control voltage of the four stages is 10kV:
The first step is a preheating stage, wherein the current is added to 10mA, and the preheating stage waits for 30 seconds;
the second step is a premelting stage, wherein the current is added to 30mA, and the waiting time is 30 seconds;
the third step is the evaporation source melting stage, the current is added to 40mA, and the waiting time is 30 seconds;
The fourth step is a stable evaporation stage, which is to determine a power stabilizing process according to a set evaporation rate: and (3) adding the current to 50mA, waiting for 30 seconds, opening a baffle after the power is stable, starting an evaporation process, and observing the evaporation rate from rising to stable evaporation in the evaporation coating process, wherein the evaporation rate is stable at a set evaporation rate. After the baffle plate is opened, the speed is rapidly increased to 40A/s, and then the current is reduced to 15mA, so that the evaporation speed is stabilized at 30A/s, and the thickness of the coating film is 4 mu m.
Example 2
The only difference from example 1 is that: the steady evaporation phase eventually stabilizes the evaporation at a rate of 40 a/s.
Example 3
The only difference from example 1 is that: the steady evaporation phase eventually stabilizes the evaporation at a rate of 20 a/s.
Comparative example 1
The only difference from example 1 is that: the silver metal material is directly placed in the red copper crucible without adding a molybdenum crucible.
In the molybdenum crucible in the embodiment 1, the evaporation power in the evaporation stage is stabilized at 1-2W under the same condition, and the means for controlling the power is to adjust the current to be 0.1-0.2mA; the red copper crucible in comparative example 1 was stabilized at an evaporation power of 300 to 500W in the same condition, and the means for controlling the power was to adjust the current to 30 to 50mA. The same applies to the above: on the premise of the evaporation rate of 30A/s, the current is used for representing the evaporation power, the evaporation power of the molybdenum crucible is 0.1-0.2mA, and the evaporation power of the red copper crucible is 30-50mA.
The evaporation source material replacement frequency was different between example 1 and comparative example 1, and the molybdenum crucible was replaced about once for the evaporation material 200 furnace (replaced together with the molybdenum crucible) in the same case, and about once for the evaporation material 30 furnace (replaced only for the silver source) in the same case of the red copper crucible. The cost of the molybdenum crucible is 200 yuan/one, the cost of silver is 10 yuan/gram, and the cost of changing 100 grams per gram is 1000 yuan. Comparative example 1 the evaporation 200 furnace was replaced about 6 more times than in example 1, which can save about 6000 yuan for example 1.
Example 1 and comparative example 1 were different in sputtering source frequency, and example 1 was used with a molybdenum crucible having zero sputtering source; the red copper crucible of comparative example 1 necessarily generates sputtering source per 1-30 furnaces, and the loss per furnace is about 50 sheets/furnace×500 yuan/sheet=25000 yuan/furnace, in the case of the 4 inch wafer with the lowest cost, and the loss per furnace of the processing equipment and the like is about 3 ten thousand yuan.
Comparative example 2
The only difference from example 1 is that: the molybdenum crucible is replaced by a tungsten crucible, and the shape and the size are unchanged.
Comparative example 3
The only difference from example 1 is that: the molybdenum crucible is replaced by a graphite crucible, and the shape and the size are unchanged.
The results show that after the tungsten crucible is replaced in comparative example 2, the crucible is cracked and the process cannot be performed every time the 2-5 furnaces are used. Comparative example 3 after replacing the graphite crucible, the crucible was cracked using 1 furnace and the process could not be continued. This is probably due to the fact that tungsten and graphite materials, although resistant to high temperatures, have poor ductility and the evaporation process is difficult to control; when the evaporation power is slightly higher, the metal materials are all melted, and tungsten and graphite materials are broken under the direct bombardment of electron beams for a long time.
Comparative example 4
The only difference from example 1 is that: the steady evaporation phase eventually stabilizes the evaporation at a rate of 15 a/s.
Comparative example 5
The only difference from example 1 is that: the evaporation procedure was not carried out according to the stages of example 1, and is specifically as follows: setting the evaporation rate to be 30A/s, directly opening a baffle plate in the evaporation stage, starting evaporation, starting no rate, rapidly increasing the current, and gradually stabilizing the evaporation rate from 0-30A/s along with the increase of the current. When the evaporation rate stabilizes at 30 a/s, the current also stabilizes.
The results show that the evaporation process of comparative example 5 has poor adhesion of metal to the wafer and easy peeling of metal because the initial evaporation rate is small.
Results discussion of examples and comparative examples:
(1) Whether sputtering source phenomenon occurs in the coating process in the example 1 and the comparative example 1 is observed, and the result shows that: in example 1, the evaporation 1000 furnace was counted, and no splash phenomenon occurred.
(2) The stable power of the coating process in example 1 and comparative example 1 was observed, and the results showed that:
In the embodiment 1, the evaporation power of the molybdenum crucible is stabilized between 0.1 and 0.2W, the 1000 furnaces are counted in the stable power, the molybdenum crucible is replaced every 200 furnaces, and when the molybdenum crucible is evaporated beyond 220 furnaces, the power is increased unstably, and the sputtering source phenomenon is easy to occur, so that the 200 furnaces are used for replacing the molybdenum crucible once. Example 1 an evaporation furnace 1000, in which a molybdenum crucible was replaced 5 times during the evaporation process, no sputtering source phenomenon occurred, and the evaporation stability of the molybdenum crucible was 100%.
Comparative example 1 evaporation was performed directly using a red copper crucible, and the evaporation power was stabilized at 300-500W. In the evaporation process of comparative example 1, sputtering source phenomenon must appear in every 1-30 furnaces, so that the silver source needs to be replaced every 30 furnaces in comparative example 1, the silver source needs to be replaced every 33 times in the evaporation process of 1000 furnaces, 4 sputtering sources appear in every 100 furnaces on average, and the stable ratio is 96%.
(3) Fig. 2 is a view of the wafer surface after sputtering of comparative example 1 and comparative example 2, wherein (a) in fig. 2 shows a view after sputtering of the red copper crucible of comparative example 1, and (b) in fig. 2 shows a view after sputtering of the tungsten crucible of comparative example 2. It can be seen that the wafers obtained in comparative examples 1 and 2 have raised silver spots on the surface.
(4) The uniformity, surface brightness and silver layer compactness of the plating layers prepared in example 1 and comparative example 4 were observed. The results show that: fig. 3 (a) shows the evaporated image of example 1, with a bright and metallic surface. Fig. 3 (b) shows the graph of comparative example 4 after evaporation, and the evaporation rate is less than 20 a/s, the surface is hazy and has no metallic luster. Therefore, when the evaporation rate of the molybdenum crucible is 20-40A/s, the surface of the evaporated wafer is bright and has metallic luster, the evaporation power is stable, and zero sputtering source can be realized.
In summary, the embodiment of the invention provides a method for evaporating silver metal for vacuum coating, which has the following advantages: (1) The molybdenum crucible is not easy to oxidize at high temperature, and can reduce the formation of impurities. (2) The purity of the molybdenum crucible is more than 99.9%, the density is 10.0g/cm 3-10.5g/cm3, the melting point is 2610-2630 ℃, and the molybdenum crucible is not easy to deform. (3) After the metal silver source material is melted, the metal silver source material is closely contacted with the molybdenum crucible, no air holes are formed in the metal, the melting process is heated uniformly, and the sputtering source frequency is reduced. (4) The molybdenum crucible is not in close contact with the red copper crucible, so that the heat dissipation is slower, and the evaporation power is smaller under the same evaporation condition compared with the red copper crucible.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. A method for evaporating and vacuum plating silver metal, which is characterized by comprising the following steps: placing a molybdenum crucible into a crucible of an evaporation device, taking the molybdenum crucible as a container for evaporating and coating silver metal materials, and forming a metal film layer on a substrate by an evaporating vacuum coating method;
The evaporation vacuum coating process comprises a preheating stage, a premelting stage, an evaporation source melting stage and a stable evaporation stage which are sequentially carried out;
The voltages applied by the preheating stage, the premelting stage, the evaporation source melting stage and the stable evaporation stage are all 9kV-11kV, and the current applied from the preheating stage to the evaporation source melting stage is gradually increased;
and in the stable evaporation stage, 48mA-52mA current is firstly applied for 20s-40s, the baffle is opened to start the evaporation process after the evaporation source material is completely melted, the current is reduced to 10mA-20mA, and the silver metal evaporation rate is controlled to be stabilized at 20A/s-40A/s.
2. The method according to claim 1, characterized in that during the preheating phase, the applied current is controlled to be 8mA-12mA and the current application time is controlled to be 20s-40s.
3. The method according to claim 1, wherein in the premelting stage, the applied current is controlled to be 28mA-32mA and the current application time is controlled to be 20s-40s.
4. The method according to claim 1, wherein the applied current is controlled to be 38mA-42mA and the current application time is controlled to be 20s-40s in the evaporation source melting stage.
5. The method according to claim 1, wherein the vacuum degree is controlled to be (1-3) ×10 -6 torr during the evaporation of the vacuum plating.
6. The method of claim 1, wherein the molybdenum crucible has a purity of greater than 99.9%, a density of 10.0g/cm 3-10.5g/cm3, and a melting point of 2610 ℃ to 2630 ℃.
7. The method of claim 1, wherein the silver metallic material has a purity of greater than 99.99%, a density of 10.3g/cm 3-10.7g/cm3, and a melting point of 951 ℃ to 971 ℃.
8. The method of claim 1, wherein the crucible of the evaporation apparatus is a red copper crucible.
9. The method of claim 1, wherein the substrate is a wafer.
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