CN117604469A - Method for plating color of semiconductor crystal - Google Patents
Method for plating color of semiconductor crystal Download PDFInfo
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- CN117604469A CN117604469A CN202311530704.5A CN202311530704A CN117604469A CN 117604469 A CN117604469 A CN 117604469A CN 202311530704 A CN202311530704 A CN 202311530704A CN 117604469 A CN117604469 A CN 117604469A
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- 239000004065 semiconductor Substances 0.000 title claims abstract description 42
- 239000013078 crystal Substances 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 28
- 238000007747 plating Methods 0.000 title claims abstract description 24
- 238000004544 sputter deposition Methods 0.000 claims abstract description 88
- 239000007789 gas Substances 0.000 claims abstract description 42
- 239000012495 reaction gas Substances 0.000 claims abstract description 24
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000010936 titanium Substances 0.000 claims abstract description 20
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 20
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 15
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000004040 coloring Methods 0.000 claims abstract description 10
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 9
- 229910010413 TiO 2 Inorganic materials 0.000 claims abstract description 9
- 239000002131 composite material Substances 0.000 claims abstract description 6
- 239000010408 film Substances 0.000 claims description 69
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 56
- 238000000151 deposition Methods 0.000 claims description 44
- 230000008021 deposition Effects 0.000 claims description 44
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 30
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 29
- 239000001301 oxygen Substances 0.000 claims description 29
- 229910052760 oxygen Inorganic materials 0.000 claims description 29
- 229910052786 argon Inorganic materials 0.000 claims description 28
- 229910052757 nitrogen Inorganic materials 0.000 claims description 15
- 239000013077 target material Substances 0.000 claims description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- 238000004140 cleaning Methods 0.000 claims description 7
- 239000012528 membrane Substances 0.000 claims description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 6
- 230000001276 controlling effect Effects 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000011248 coating agent Substances 0.000 claims description 5
- 238000000576 coating method Methods 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 229910003460 diamond Inorganic materials 0.000 claims description 5
- 239000010432 diamond Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
- 239000010453 quartz Substances 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000010409 thin film Substances 0.000 claims description 4
- 238000009500 colour coating Methods 0.000 claims description 3
- 229910002601 GaN Inorganic materials 0.000 claims description 2
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 claims description 2
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 2
- 230000001678 irradiating effect Effects 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 2
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 2
- 239000003086 colorant Substances 0.000 abstract description 9
- 230000007797 corrosion Effects 0.000 abstract description 3
- 238000005260 corrosion Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 101001018064 Homo sapiens Lysosomal-trafficking regulator Proteins 0.000 abstract description 2
- 102100033472 Lysosomal-trafficking regulator Human genes 0.000 abstract description 2
- 235000010703 Modiola caroliniana Nutrition 0.000 abstract description 2
- 244000038561 Modiola caroliniana Species 0.000 abstract description 2
- 239000010410 layer Substances 0.000 description 12
- 239000000758 substrate Substances 0.000 description 12
- 238000005086 pumping Methods 0.000 description 9
- 239000000498 cooling water Substances 0.000 description 6
- 238000004806 packaging method and process Methods 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 6
- 235000012431 wafers Nutrition 0.000 description 6
- 230000003749 cleanliness Effects 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 230000003746 surface roughness Effects 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000002356 single layer Substances 0.000 description 3
- 238000005477 sputtering target Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000000007 visual effect Effects 0.000 description 2
- 241000282414 Homo sapiens Species 0.000 description 1
- 206010048245 Yellow skin Diseases 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000000089 atomic force micrograph Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- FDZZZRQASAIRJF-UHFFFAOYSA-M malachite green Chemical compound [Cl-].C1=CC(N(C)C)=CC=C1C(C=1C=CC=CC=1)=C1C=CC(=[N+](C)C)C=C1 FDZZZRQASAIRJF-UHFFFAOYSA-M 0.000 description 1
- 229940107698 malachite green Drugs 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- MCPLVIGCWWTHFH-UHFFFAOYSA-L methyl blue Chemical compound [Na+].[Na+].C1=CC(S(=O)(=O)[O-])=CC=C1NC1=CC=C(C(=C2C=CC(C=C2)=[NH+]C=2C=CC(=CC=2)S([O-])(=O)=O)C=2C=CC(NC=3C=CC(=CC=3)S([O-])(=O)=O)=CC=2)C=C1 MCPLVIGCWWTHFH-UHFFFAOYSA-L 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 230000001902 propagating effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001771 vacuum deposition 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
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
-
- 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
- C23C14/0015—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterized by the colour of the layer
-
- 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
- C23C14/0641—Nitrides
-
- 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
- C23C14/08—Oxides
- C23C14/083—Oxides of refractory metals or yttrium
-
- 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
- C23C14/10—Glass or silica
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
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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 belongs to the field of semiconductor surface coloring, and relates to a method for coloring semiconductor crystals. Round titanium targets with purity of 99.8% are selected, and high-purity Ar is used as sputtering discharge gas and high-purity N 2 Or O 2 As active reaction gas, a TiN film and TiO film with rich colors can be deposited on the semiconductor crystal by a magnetron sputtering method 2 /SiO 2 /TiO 2 Composite dielectric films including silvery white, violet, blue, green, yellow, orange, mauve, and intermediate colors thereof; the color-changing production flexibility is strong, the plating layer is hard and compact, and the plating layer is wear-resistant and corrosion-resistant, and compared with the colors presented by other methods, the color produced by the method is more stable, durable, vivid and bright and is difficult to damage.
Description
Technical Field
The invention belongs to the field of semiconductor surface coloring, and relates to a method for coloring semiconductor crystals.
Background
White light is a mixed light that contains light of multiple wavelengths of red, orange, yellow, green, blue and violet. The refractive indices of the different substances are different and light is partially reflected as it passes through the interface between the two substances. When the thickness of the two films meets a specific relation, light in a certain frequency range can be completely reflected back, so that a specific visual color is generated. From an optical perspective, light is partially reflected each time it passes through the interface between two layers, and in a periodic multilayer film, many of the reflected beams interfere with each other. The absorption of light by the dielectric multilayer film is typically small and light of certain colors propagating forward is reflected, which creates color. By utilizing the principle of color generation, people design color lenses, color glass, color crystal jewelry and the like. Devices for reflecting X-rays, infrared light and even microwaves are designed aiming at different electromagnetic wave wavelengths.
At present, the surface coloring is mainly to coat metal, metal oxide and the like on the surface of glass to form transparent, semitransparent or opaque color coating, and the preparation method mainly comprises a vacuum coating method, a sol-gel method and the like. SiO produced by the sol-gel process 2 -TiO 2 Adding coloring agents such as aurous amine yellow, malachite green, methyl blue and the like into the sol to form the color nano transparent film. However, the preparation method has single film color, complex raw material preparation and higher environmental requirements. With the continuous improvement of the living standard of human beings, the aesthetic pursuit of people is also higher and higher, and the single color no longer meets the requirements of most people.
Therefore, there is a need to develop a method for plating a multicolor semiconductor crystal with various film colors and simple method.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for plating the color of a semiconductor crystal.
The invention is realized by the following technical scheme:
a method for plating color of semiconductor crystal includes enabling target material to react on semiconductor crystal to form color plating film under action of sputtering discharge gas and active reaction gas through magnetron sputtering; the flow ratio of the sputtering discharge gas to the active reaction gas is (1-20): 1, the working voltage is set to 0.5-2.0Pa, and the sputtering power is 20-200W during the thin film sputtering deposition.
According to the present invention, preferably, the semiconductor crystal is a polished silicon, silicon carbide, gallium nitride, diamond or aluminum nitride semiconductor crystal.
According to the invention, preferably, the magnetron sputtering adopts a titanium target or quartz as a target material, argon as a sputtering discharge gas and nitrogen or oxygen as an active reaction gas.
According to a further preferred aspect of the present invention, the magnetron sputtering is performed by sputtering a TiN film using a titanium target with argon as a sputtering discharge gas and nitrogen as an active reaction gas.
According to a further preferred embodiment of the present invention, the magnetron sputtering sequentially uses high purity titanium, high purity quartz, high purity titanium as a target material, argon as a sputtering discharge gas, oxygen as an active reaction gas, and sputtering TiO 2 /SiO 2 /TiO 2 A composite dielectric film.
According to still further preferred embodiments of the present invention, the method for coloring a semiconductor crystal comprises the steps of:
(1) Sequentially placing the semiconductor crystal into acetone, absolute ethyl alcohol and deionized water, carrying out ultrasonic heating and cleaning at 60-80 ℃, then drying by using nitrogen, and then irradiating for 5 minutes by using oxygen plasma to obtain a pretreated semiconductor crystal; the surface quality and cleanliness of the substrate can directly influence the quality of the formed film;
(2) Placing the pretreated semiconductor crystal in magnetron sputtering coating equipment, introducing sputtering discharge gas argon into a sputtering chamber, pre-sputtering, introducing active reaction gas into the sputtering chamber, controlling the flow ratio of the sputtering discharge gas to the active reaction gas by using a gas flowmeter, regulating working voltage and sputtering power, switching on a power supply, sputtering a target material, and finishing the color coating.
The surface of the semiconductor crystal after the pretreatment in the step (1) must be dry and dust-free, and require a plasma irradiation treatment.
According to the present invention, preferably, in the step (2), the target is titanium, the active reaction gas is nitrogen, and the sputtering parameters are: the flow ratio of argon to nitrogen was 21:8, setting the working voltage to 0.8Pa, the sputtering power to 64W and the deposition time to 10-50min.
According to a preferred embodiment of the present invention, in the step (2): firstly, when a titanium target is used as a target material and active reaction gas is oxygen, setting sputtering parameters: the flow ratio of argon to oxygen was 15:1, setting the working voltage to be 1.0Pa, setting the sputtering power to be 40-60W, switching on a direct current power supply, starting the deposition of the gas discharge film, and completing the first layer of TiO after the deposition time is 10-50min 2 A membrane; and then the flow ratio of argon to oxygen is adjusted to 27:3, setting the working voltage to 2.0Pa, setting the sputtering power to 150-180W, switching on the radio frequency power supply, starting the deposition of the gas discharge film, and completing the SiO after the deposition for 10-50min 2 Sputtering of the film;
finally, the flow ratio of argon to oxygen is adjusted back to 15:1, setting the working voltage to be 1.0Pa, adjusting the sputtering power to be 40W, switching on a direct current power supply after the sputtering power is a preset value, starting the deposition of the gas discharge film, and completing the deposition of another layer of TiO after the deposition time is 10-50min 2 And (3) a film.
Compared with the prior art, the invention has the following technical effects: the magnetron sputtering coating production process is simple, and the prepared TiN and TiO are prepared 2 /SiO 2 The composite dielectric film has rich color, strong flexibility in color changing production, hard and compact plating layer, wear resistance and corrosion resistance, and compared with the colors presented by other methods, the color produced by the method is more stable, durable, bright and difficult to damage.
Drawings
Fig. 1 is a film structure diagram of a TiN film of the present invention which is colored on a Mo Sang diamond.
FIG. 2 shows TiO according to the invention 2 /SiO 2 The alternating dielectric films are patterned on a Mo Sang diamond in a film system.
FIG. 3 is a diagram showing the semiconductor crystal of example 1 of the present invention before (a) and after (b) the plating.
Fig. 4 is a physical diagram of the semiconductor of example 2 of the present invention after the plating of the color.
Fig. 5 is an X-ray diffraction pattern of TiN plating layer of example 1 of the present invention.
Fig. 6 is an AFM image of TiN plating of example 1 of the present invention.
FIG. 7 is a single layer thin film deposited on a silicon wafer according to a comparative example of the present invention; (a) (b) is TiO 2 The film (c) and (d) are SiO 2 A film.
Detailed Description
The present invention will be further described with reference to examples, but the scope of the present invention is not limited thereto.
The color of the plating film is different on the surface of the semiconductor due to the different material and thickness of the plating film. The color and thickness of a single-layer coating film or a composite dielectric film on the surface of a colorless semiconductor crystal are shown in table 1.
TABLE 1 color and thickness of coating film on the surface of colorless semiconductor crystal
Example 1
A method of coloring yellow on a morse diamond comprising the steps of:
(1) Pretreatment of a substrate: the surface quality and cleanliness of the base can have a direct impact on the quality of the film formed, including film adhesion to the substrate, film surface roughness, brightness, etc. Selecting a colorless transparent Mo Sangzuan as a deposition substrate, sequentially placing the deposition substrate into acetone, absolute ethyl alcohol and deionized water, carrying out ultrasonic heating and cleaning at 60-80 ℃ for 15min, and drying by using nitrogen. Then oxygen plasma is irradiated for 5 minutes to increase the wettability.
(2) Preparation before starting up: the main power supply is turned on, cooling water is turned on, the temperature is 25 ℃, and the smooth flow of each waterway is ensured; checking whether the flow valve, the rough pumping valve, the gate valve and the like are all in a closed state; the pretreated semiconductor wafer is mounted on a sample stage.
(3) Vacuumizing in a vacuum chamber: after the whole sample stage is lowered into the sputtering chamber, a mechanical pump is started to vacuumize, a side pumping valve is opened, the side pumping valve is closed after the pressure is lowered to 3-5Pa, an electromagnetic valve is opened, and a molecular pump is started to vacuumize until the vacuum degree is lower than 2 multiplied by 10 -4 Pa, the value is the vacuum degree of the whole experiment.
(4) Pre-sputter cleaning of titanium targets: closing ionization, closing a baffle in front of the target, introducing working gas argon into a sputtering chamber, starting a direct current power supply, and pre-sputtering the target for 15min after starting, wherein the glow is light blue. The pre-sputtering target material can effectively remove impurities such as oxides, organic matters and the like on the surface of the pure titanium target.
(5) Film sputtering deposition: introducing reaction gas nitrogen into the sputtering chamber, and controlling the flow ratio of the nitrogen to the argon to be 21 by using a gas flowmeter: 8, setting the working voltage to be 0.8Pa, adjusting the sputtering power to be 64W, switching on a direct current power supply, starting the deposition of the gas discharge film, and performing the deposition for 30min, wherein the glow is pink. The finally obtained plated semiconductor crystal is yellow.
(6) And (3) sputtering post-treatment: after sputtering, closing a gate valve, closing a molecular pump, closing a solenoid valve after parameters are not displayed on a dial of a controller on the molecular pump, closing the pump, breaking vacuum, taking out a sample, closing the pump, closing cooling water and closing a power supply. And (5) independently packaging the prepared sample in a clean sample box for packaging and preserving.
The figure of the Mo Sang drill before and after the plating is shown in fig. 3, a is Mo Sang drill before the non-plating, and b is Mo Sang drill after the plating.
XRD analysis was performed on the TiN film layer on the Mo Sang drill, and the results are shown in fig. 5:
the TiN film layer deposited by magnetron sputtering has two characteristic peaks at 36 degrees and 41 degrees, which are respectively considered as a (111) orientation diffraction peak and a (200) orientation diffraction peak of face-centered cubic TiN, and the strongest peak is (111), and a certain preferred orientation of the (111) face exists because the (111) face is the closest packed face, the free energy is minimum, the relative growth is faster, and the preferred growth orientation is easy to occur.
AFM analysis was performed on the TiN film layer on the Mo Sang drill, and the results are shown in fig. 6:
the surface roughness and the root mean square roughness of the TiN film layer deposited by magnetron sputtering are smaller, and the surface structure is compact, smooth and compact.
Example 2
A method of coloring a morse drill to pink comprising the steps of:
(1) Pretreatment of a substrate: the surface quality and cleanliness of the base can have a direct impact on the quality of the film formed, including film adhesion to the substrate, film surface roughness, brightness, etc. Selecting a colorless transparent Mo Sangzuan as a deposition substrate, sequentially placing the deposition substrate into acetone, absolute ethyl alcohol and deionized water, carrying out ultrasonic heating and cleaning at 60-80 ℃ for 15min, and drying by using nitrogen. Then oxygen plasma is irradiated for 5 minutes to increase the wettability.
(2) Preparation before starting up: the main power supply is turned on, cooling water is turned on, the temperature is 25 ℃, and the smooth flow of each waterway is ensured; checking whether the flow valve, the rough pumping valve, the gate valve and the like are all in a closed state; the pretreated semiconductor wafers are sequentially mounted on a sample stage.
(3) Vacuumizing in a vacuum chamber: after the whole sample stage is lowered into the sputtering chamber, a mechanical pump is started to vacuumize, a side pumping valve is opened, the side pumping valve is closed after the pressure is lowered to 3-5Pa, an electromagnetic valve is opened, and a molecular pump is started to vacuumize until the vacuum degree is lower than 2 multiplied by 10 -4 Pa, the value is the vacuum degree of the whole experiment.
(4) Pre-sputter cleaning of titanium targets: closing ionization, closing a baffle in front of the target, introducing working gas argon into a sputtering chamber, starting a direct current power supply, and pre-sputtering the target for 15min after starting, wherein the glow is light blue. The pre-sputtering target material can effectively remove impurities such as oxides, organic matters and the like on the surface of the pure titanium target.
(5) Film sputtering deposition: introducing reaction gas oxygen into the sputtering chamber, and controlling the flow ratio of argon to oxygen to be 15 by using a gas flowmeter: 1, setting the working voltage to be 1.0Pa, adjusting the sputtering power to be 40W, then switching on a direct current power supply, starting the deposition of the gas discharge film, and completing the first layer of TiO after the deposition time is 40min 2 A membrane; then the flow ratio of argon to oxygen is adjusted to 27:3, setting working voltageSetting the pressure at 2.0Pa, adjusting the sputtering power to 170W, switching on a radio frequency power supply, starting the deposition of the gas discharge film, and completing the SiO deposition for 30min 2 Sputtering of the film; finally, the flow ratio of argon to oxygen is adjusted back to 15:1, setting the working voltage to be 1.0Pa, adjusting the sputtering power to be 40W, then switching on a direct current power supply, starting the deposition of the gas discharge film, and completing the final TiO after the deposition time is 40min 2 A membrane; the semiconductor crystal finally obtained is pink.
(6) And (3) sputtering post-treatment: after sputtering, closing a gate valve, closing a molecular pump, closing a solenoid valve after parameters are not displayed on a dial of a controller on the molecular pump, closing the pump, breaking vacuum, taking out a sample, closing the pump, closing cooling water and closing a power supply. And (5) independently packaging the prepared sample in a clean sample box for packaging and preserving.
Example 3
A method of coloring silicon yellow, comprising the steps of:
(1) Pretreatment of a substrate: the surface quality and cleanliness of the base can have a direct impact on the quality of the film formed, including film adhesion to the substrate, film surface roughness, brightness, etc. Silicon wafers are selected as a deposition substrate, sequentially put into acetone, absolute ethyl alcohol and deionized water, heated and cleaned for 15min at 60-80 ℃ by ultrasonic, and dried by nitrogen. Then oxygen plasma is irradiated for 5 minutes to increase the wettability.
(2) Preparation before starting up: the main power supply is turned on, cooling water is turned on, the temperature is 25 ℃, and the smooth flow of each waterway is ensured; checking whether the flow valve, the rough pumping valve, the gate valve and the like are all in a closed state; the pretreated semiconductor wafers are sequentially mounted on a sample stage.
(3) Vacuumizing in a vacuum chamber: after the whole sample stage is lowered into the sputtering chamber, a mechanical pump is started to vacuumize, a side pumping valve is opened, the side pumping valve is closed after the pressure is lowered to 3-5Pa, an electromagnetic valve is opened, and a molecular pump is started to vacuumize until the vacuum degree is lower than 2 multiplied by 10 -4 Pa, the value is the vacuum degree of the whole experiment.
(4) Pre-sputter cleaning of titanium targets: closing ionization, closing a baffle in front of the target, introducing working gas argon into a sputtering chamber, starting a direct current power supply, and pre-sputtering the target for 15min after starting, wherein the glow is light blue. The pre-sputtering target material can effectively remove impurities such as oxides, organic matters and the like on the surface of the pure titanium target.
(5) Film sputtering deposition: introducing reaction gas oxygen into the sputtering chamber, and controlling the flow ratio of argon to oxygen to be 15 by using a gas flowmeter: 1, setting the working voltage to be 1.0Pa, adjusting the sputtering power to be 50W, then switching on a direct current power supply, starting the deposition of the gas discharge film, and completing the first layer of TiO after the deposition time is 20min 2 A membrane; then the flow ratio of argon to oxygen is adjusted to 27:3, setting the working voltage to 2.0Pa, adjusting the sputtering power to 150W, switching on a radio frequency power supply, starting the deposition of the gas discharge film, and completing the SiO deposition for 30min 2 Sputtering of the film; finally, the flow ratio of argon to oxygen is adjusted back to 15:1, setting the working voltage to be 1.0Pa, adjusting the sputtering power to be 40W, then switching on a direct current power supply, starting the deposition of the gas discharge film, and completing the final TiO after the deposition time is 20min 2 A membrane; the semiconductor crystal finally obtained is yellow.
(6) And (3) sputtering post-treatment: after sputtering, closing a gate valve, closing a molecular pump, closing a solenoid valve after parameters are not displayed on a dial of a controller on the molecular pump, closing the pump, breaking vacuum, taking out a sample, closing the pump, closing cooling water and closing a power supply. And (5) independently packaging the prepared sample in a clean sample box for packaging and preserving.
Comparative example:
compared with example 3, the difference is that the thin film sputter deposition portion of step (5):
introducing reaction gas oxygen into the sputtering chamber, and controlling the flow ratio of argon to oxygen to be 15 by using a gas flowmeter: 1, setting the working voltage to be 1.0Pa, adjusting the sputtering power to be 40W, switching on a direct current power supply after the sputtering power is a preset value, starting the deposition of the gas discharge film, and completing the TiO after the deposition time is 50min 2 A membrane;
introducing reaction gas oxygen into the sputtering chamber, and then adjusting the flow ratio of argon to oxygen to 27 by using a gas flowmeter: 3, setting the working voltage to 2.0Pa, adjusting the sputtering power to 170W, and switching on after the sputtering power is a preset valueA radio frequency power supply, the deposition of the gas discharge film is started, the deposition time is 40min, and the SiO is completed 2 Sputtering of the film;
the sputtered sample is shown in FIG. 7, and a single layer of TiO is known 2 Or SiO 2 The film was colorless on the silicon wafer. In example 3, however, when TiO 2 And SiO 2 When alternating dielectric films are formed, light in a certain frequency range can be totally reflected back, thereby generating a specific visual color.
The invention selects round titanium targets with purity of 99.8 percent, ar with purity of 99.99 percent as sputtering discharge gas and N 2 Or O 2 As active reaction gas, a TiN film and TiO film with rich colors can be deposited on the semiconductor crystal by a magnetron sputtering method 2 /SiO 2 /TiO 2 Composite dielectric films including silvery white, violet, blue, green, yellow, orange, mauve, and intermediate colors thereof; the process parameters for preparing the TiN yellow film are the most stable and the comprehensive performance is the best through a large number of experiments, such as hard and compact plating layer, high brightness, wear resistance, corrosion resistance and the like.
Claims (8)
1. A method for plating color of semiconductor crystal is characterized in that a target material reacts on the semiconductor crystal to form a color plating film under the action of sputtering discharge gas and active reaction gas by magnetron sputtering; the flow ratio of the sputtering discharge gas to the active reaction gas is (1-20): 1, the working voltage is set to 0.5-2.0Pa, and the sputtering power is 20-200W during the thin film sputtering deposition.
2. The method for coloring a semiconductor crystal according to claim 1, wherein the semiconductor crystal is a polished silicon, silicon carbide, gallium nitride, diamond or aluminum nitride semiconductor crystal.
3. The method according to claim 1, wherein the magnetron sputtering uses a titanium target or quartz as a target material, argon as a sputtering discharge gas, and nitrogen or oxygen as an active reaction gas.
4. The method for plating a semiconductor crystal according to claim 3, wherein the magnetron sputtering is performed by sputtering a TiN film using a titanium target and using argon as a sputtering discharge gas and nitrogen as an active reaction gas.
5. The method for plating a semiconductor crystal according to claim 3, wherein the magnetron sputtering sequentially uses high purity titanium, high purity quartz, high purity titanium as a target, argon as a sputtering discharge gas, oxygen as an active reaction gas, and sputtering TiO 2 /SiO 2 /TiO 2 A composite dielectric film.
6. The method for plating color of a semiconductor crystal according to claim 4 or 5, comprising the steps of:
(1) Sequentially placing the semiconductor crystal into acetone, absolute ethyl alcohol and deionized water, ultrasonically cleaning at 60-80 ℃, then drying by using nitrogen, and then irradiating for 5 minutes by using oxygen plasma to obtain a pretreated semiconductor crystal;
(2) Placing the pretreated semiconductor crystal in magnetron sputtering coating equipment, introducing sputtering discharge gas argon into a sputtering chamber, pre-sputtering, introducing active reaction gas into the sputtering chamber, controlling the flow ratio of the sputtering discharge gas to the active reaction gas by using a gas flowmeter, regulating working voltage and sputtering power, switching on a power supply, sputtering a target material, and finishing the color coating.
7. The method of claim 6, wherein the target in the step (2) is titanium, the reactive gas is nitrogen, and the sputtering parameters are as follows: the flow ratio of argon to nitrogen was 21:8, setting the working voltage to 0.8Pa, the sputtering power to 64W and the deposition time to 10-50min.
8. The method for coloring semiconductor crystals according to claim 6, wherein said step2) In (a): firstly, when a titanium target is used as a target material and active reaction gas is oxygen, setting sputtering parameters: the flow ratio of argon to oxygen was 15:1, setting the working voltage to be 1.0Pa, setting the sputtering power to be 40-60W, switching on a direct current power supply, starting the deposition of the gas discharge film, and completing the first layer of TiO after the deposition time is 10-50min 2 A membrane; and then the flow ratio of argon to oxygen is adjusted to 27:3, setting the working voltage to 2.0Pa, setting the sputtering power to 150-180W, switching on the radio frequency power supply, starting the deposition of the gas discharge film, and completing the SiO after the deposition for 10-50min 2 Sputtering of the film;
finally, the flow ratio of argon to oxygen is adjusted back to 15:1, setting the working voltage to be 1.0Pa, adjusting the sputtering power to be 40W, switching on a direct current power supply after the sputtering power is a preset value, starting the deposition of the gas discharge film, and completing the deposition of another layer of TiO after the deposition time is 10-50min 2 And (3) a film.
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