CN115093903A - Cleaning agent and application thereof, cleaning method of thin film circuit board substrate and preparation method of thin film circuit board - Google Patents
Cleaning agent and application thereof, cleaning method of thin film circuit board substrate and preparation method of thin film circuit board Download PDFInfo
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- CN115093903A CN115093903A CN202210849130.7A CN202210849130A CN115093903A CN 115093903 A CN115093903 A CN 115093903A CN 202210849130 A CN202210849130 A CN 202210849130A CN 115093903 A CN115093903 A CN 115093903A
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- 239000000758 substrate Substances 0.000 title claims abstract description 102
- 239000012459 cleaning agent Substances 0.000 title claims abstract description 93
- 239000010409 thin film Substances 0.000 title claims abstract description 93
- 238000004140 cleaning Methods 0.000 title claims abstract description 61
- 238000000034 method Methods 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 85
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 68
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 50
- 150000007522 mineralic acids Chemical class 0.000 claims abstract description 41
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 36
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 34
- 239000010408 film Substances 0.000 claims abstract description 20
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000004094 surface-active agent Substances 0.000 claims abstract description 15
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 25
- 238000001035 drying Methods 0.000 claims description 16
- RYYKJJJTJZKILX-UHFFFAOYSA-M sodium octadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC([O-])=O RYYKJJJTJZKILX-UHFFFAOYSA-M 0.000 claims description 7
- NWZBFJYXRGSRGD-UHFFFAOYSA-M sodium;octadecyl sulfate Chemical compound [Na+].CCCCCCCCCCCCCCCCCCOS([O-])(=O)=O NWZBFJYXRGSRGD-UHFFFAOYSA-M 0.000 claims description 7
- 238000009472 formulation Methods 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 239000010453 quartz Substances 0.000 abstract description 57
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 57
- 239000002184 metal Substances 0.000 abstract description 13
- 229910052751 metal Inorganic materials 0.000 abstract description 13
- 238000005240 physical vapour deposition Methods 0.000 abstract description 11
- 239000000853 adhesive Substances 0.000 abstract description 6
- 230000001070 adhesive effect Effects 0.000 abstract description 6
- 238000005530 etching Methods 0.000 abstract description 6
- 238000001259 photo etching Methods 0.000 abstract description 6
- 238000013329 compounding Methods 0.000 abstract description 3
- 230000001276 controlling effect Effects 0.000 abstract description 3
- 239000003344 environmental pollutant Substances 0.000 abstract description 3
- 231100000719 pollutant Toxicity 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 230000001105 regulatory effect Effects 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 11
- 238000012360 testing method Methods 0.000 description 11
- 238000012545 processing Methods 0.000 description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- 229920002313 fluoropolymer Polymers 0.000 description 6
- 239000011521 glass Substances 0.000 description 6
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 6
- 230000002378 acidificating effect Effects 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 229910001873 dinitrogen Inorganic materials 0.000 description 3
- 238000011068 loading method Methods 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- 238000004891 communication Methods 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 1
- 239000007853 buffer solution Substances 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- -1 polypropylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/37—Mixtures of compounds all of which are anionic
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/08—Cleaning involving contact with liquid the liquid having chemical or dissolving effect
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
- B08B3/12—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration by sonic or ultrasonic vibrations
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/04—Water-soluble compounds
- C11D3/042—Acids
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/04—Water-soluble compounds
- C11D3/046—Salts
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/20—Organic compounds containing oxygen
- C11D3/2003—Alcohols; Phenols
- C11D3/2006—Monohydric alcohols
- C11D3/201—Monohydric alcohols linear
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/39—Organic or inorganic per-compounds
- C11D3/3942—Inorganic per-compounds
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/22—Secondary treatment of printed circuits
- H05K3/26—Cleaning or polishing of the conductive pattern
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/04—Carboxylic acids or salts thereof
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/02—Anionic compounds
- C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
- C11D1/14—Sulfonic acids or sulfuric acid esters; Salts thereof derived from aliphatic hydrocarbons or mono-alcohols
- C11D1/146—Sulfuric acid esters
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Microelectronics & Electronic Packaging (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Emergency Medicine (AREA)
- Cleaning By Liquid Or Steam (AREA)
Abstract
The invention belongs to the technical field of integrated circuits, and particularly relates to a cleaning agent and application thereof, a cleaning method of a thin film circuit board substrate and a preparation method of the thin film circuit board. The cleaning agent provided by the invention comprises the following components in percentage by mass: 1-5% of ammonium fluoride, 3-10% of inorganic acid, 5-10% of hydrogen peroxide, 10-20% of ethanol, 0.1-1% of surfactant and the balance of water; the inorganic acid comprises hydrofluoric acid and/or phosphoric acid. The cleaning agent provided by the invention is prepared by compounding ammonium fluoride, hydrofluoric acid and/or phosphoric acid, hydrogen peroxide, ethanol, a surfactant and water, and regulating and controlling the cleaning agent obtained by the raw materials in the range, so that pollutants attached to the surface of a quartz substrate can be effectively removed, the adhesive force of methods such as physical vapor deposition, photoetching or etching and the like in the process of preparing a metal film on the surface of a quartz substrate is improved, and the phenomenon that the metal film falls off from the surface of the quartz substrate is effectively avoided by the finally processed film circuit board.
Description
Technical Field
The invention belongs to the technical field of integrated circuits, and particularly relates to a cleaning agent and application thereof, a cleaning method of a thin film circuit board substrate and a preparation method of the thin film circuit board.
Background
The quartz crystal has the characteristics of high temperature resistance, low expansion coefficient, good thermal shock resistance, high chemical stability, good electrical insulation performance, high dielectric constant stability, small dielectric loss tangent, excellent high-frequency performance and the like, and a thin film circuit processed by the quartz crystal substrate is more and more widely applied to the field of wireless communication. Particularly, as the terahertz wireless communication technology is continuously developed and applied, the application of the quartz substrate thin film circuit is rapidly increased. The quartz substrate thin film circuit is a circuit processed on the surface of a quartz substrate based on the processes of thin film integrated physical vapor deposition, photoetching, etching and the like.
A key technical problem to be solved is to improve the adhesive force between a metal film and a substrate and avoid the metal film from falling off from the surface of the substrate by depositing the metal film on a circuit substrate through a physical vapor deposition (such as magnetron sputtering) process. A commonly used method for improving the adhesion between the metal thin film and the substrate is to enhance the cleaning of the substrate before the physical vapor deposition, for example, cleaning with an inorganic acidic cleaning agent, an inorganic alkaline cleaning agent or an organic cleaning agent, and then drying. For the quartz substrate, because the surface chemical energy of the quartz substrate is high, the conventional acidic, alkaline or organic cleaning agent is difficult to remove the pollution on the surface, so that the metal film with high adhesive force is difficult to obtain on the surface of the quartz substrate during physical vapor deposition, and the phenomenon that the metal film falls off from the surface of the quartz substrate occurs in a finally processed film circuit.
Disclosure of Invention
The invention aims to provide a cleaning agent and application thereof, a cleaning method of a thin film circuit board substrate and a preparation method of the thin film circuit board.
In order to achieve the above purpose, the invention provides the following technical scheme:
the invention provides a cleaning agent, which comprises the following components in percentage by mass:
1-5% of ammonium fluoride, 3-10% of inorganic acid, 5-10% of hydrogen peroxide, 10-20% of ethanol, 0.1-1% of surfactant and the balance of water; the inorganic acid comprises hydrofluoric acid and/or phosphoric acid; the mass percentage of HF in the hydrofluoric acid is 38-40 wt%; h in the phosphoric acid 3 PO 4 The mass percentage of the component (A) is 82-85 wt%.
Preferably, the inorganic acid comprises hydrofluoric acid and phosphoric acid, and the volume percentage of the hydrofluoric acid in the inorganic acid is 10-50%.
Preferably, the surfactant comprises sodium stearyl sulfate and/or sodium stearate.
The invention provides application of the cleaning agent in the technical scheme in cleaning a thin film circuit board substrate.
The invention provides a method for cleaning a thin film circuit board substrate, which comprises the following steps:
and soaking the thin film circuit board substrate into a cleaning agent for cleaning, wherein the cleaning agent is the cleaning agent in the technical scheme.
Preferably, the temperature of the cleaning agent during cleaning is 40-60 ℃.
Preferably, the cleaning is ultrasonic cleaning, the ultrasonic frequency of the ultrasonic cleaning is 28-40 kHz, and the ultrasonic power of the ultrasonic cleaning is 100-300W.
Preferably, the ultrasonic time of the ultrasonic cleaning is 10-30 min.
The invention provides a preparation method of a thin film circuit board, which comprises the following steps:
cleaning and drying the thin film circuit board substrate according to the cleaning method of the technical scheme to obtain the cleaned thin film circuit board substrate;
and preparing a thin film circuit on the surface of the cleaned thin film circuit board substrate to obtain the thin film circuit board.
Preferably, the drying temperature is 120-200 ℃, and the drying heat preservation time is 2-4 h.
The invention provides a cleaning agent, which comprises the following components in percentage by mass: 1-5% of ammonium fluoride, 3-10% of inorganic acid, 5-10% of hydrogen peroxide, 10-20% of ethanol, 0.1-1% of surfactant and the balance of water; the inorganic acid comprises hydrofluoric acid and/or phosphoric acid; the mass percentage of HF in the hydrofluoric acid is 38-40 wt%; h in the phosphoric acid 3 PO 4 The mass percentage of the component (A) is 82-85 wt%. The cleaning agent provided by the invention is prepared by compounding ammonium fluoride, hydrofluoric acid and/or phosphoric acid, hydrogen peroxide, ethanol, a surfactant and water, and simultaneously regulating and controlling the cleaning agent obtained by the raw materials in the range, compared with a conventional acidic cleaning agent, an alkaline cleaning agent or an organic solvent cleaning agent such as acetone, ethanol and the like, the cleaning agent can effectively remove pollutants attached to the surface of a quartz substrate, so that the adhesive force of methods such as physical vapor deposition, photoetching or etching and the like in the preparation of a metal film on the surface of the quartz substrate is improved, and the phenomenon that the metal film falls off from the surface of the quartz substrate is effectively avoided by the finally processed film circuit board.
The invention provides a method for cleaning a thin film circuit board substrate, which comprises the following steps: and soaking the thin film circuit board substrate into a cleaning agent for cleaning, wherein the cleaning agent is the cleaning agent in the technical scheme. According to the invention, the substrate of the thin film circuit board is cleaned by adopting the cleaning agent in the technical scheme, so that the cleanness of the surface of the substrate can be improved, and then the thin film circuit is prepared on the surface of the substrate, so that the adhesive force of a metal film layer of the thin film circuit of the quartz substrate can be improved.
Drawings
FIG. 1 is a graph showing the test results of a quartz substrate thin film circuit board prepared in example 7 of the present invention;
fig. 2 is a graph showing the test results of the quartz substrate thin film circuit board prepared in comparative example 1 of the present invention.
Detailed Description
The invention provides a cleaning agent, which comprises the following components in percentage by mass:
1-5% of ammonium fluoride, 3-10% of inorganic acid, 5-10% of hydrogen peroxide, 10-20% of ethanol, 0.1-1% of surfactant and the balance of water; the inorganic acid comprises hydrofluoric acid and/or phosphoric acid; the mass percentage of HF in the hydrofluoric acid is 38-40 wt%; h in the phosphoric acid 3 PO 4 The content of (b) is 82-85 wt%.
In the present invention, all the preparation starting materials/components are commercially available products well known to those skilled in the art unless otherwise specified.
The cleaning agent provided by the invention comprises 1-5% of ammonium fluoride by mass percentage, and preferably 1.5-4.5%.
In the invention, the ammonium fluoride and the hydrofluoric acid form a buffer system and can activate the surface of the substrate; the phosphoric acid is used for removing inorganic pollution on the surface of the substrate; the ethanol acts to remove organic contamination from the substrate surface, and the hydrogen peroxide and the surfactant facilitate the removal of the organic contamination.
The cleaning agent provided by the invention comprises 3-10% of inorganic acid by mass percentage, and preferably 3.5-9.5%.
In the present invention, the inorganic acid includes hydrofluoric acid and/or phosphoric acid, and preferably includes hydrofluoric acid and phosphoric acid.
In the invention, the mass percentage of HF in the hydrofluoric acid is 38-40 wt%, preferably 38.5-39 wt%
In the present invention, H in the phosphoric acid 3 PO 4 The content of (b) is 82-85 wt%, preferably 82.5-84 wt%.
In the invention, the inorganic acid preferably comprises hydrofluoric acid and phosphoric acid, and the volume percentage content of the hydrofluoric acid in the inorganic acid is preferably 10-50%, and more preferably 12-45%.
The cleaning agent provided by the invention comprises 5-10% of hydrogen peroxide by mass percentage, and preferably 5.5-9%.
The cleaning agent provided by the invention comprises 10-20% of ethanol by mass percentage, and preferably 12-17.5%.
The cleaning agent provided by the invention comprises 0.1-1% of surfactant by mass percentage, and preferably 0.2-0.8%.
In the present invention, the surfactant preferably includes sodium stearyl sulfate and/or sodium stearate, and more preferably includes sodium stearyl sulfate or sodium stearate.
The cleaning agent provided by the invention comprises the balance of water in percentage by mass.
The invention has no special requirements on the preparation method of the cleaning agent, and the components are uniformly mixed.
In the present invention, the cleaning agent is preferably contained in a glass container.
The invention provides application of the cleaning agent in the technical scheme in cleaning a thin film circuit board substrate.
In the present invention, the thin film circuit board substrate is particularly preferably a quartz substrate.
The invention provides a method for cleaning a thin film circuit board substrate, which comprises the following steps:
and soaking the thin film circuit board substrate into a cleaning agent for cleaning, wherein the cleaning agent is the cleaning agent in the technical scheme.
In the present invention, it is preferable that the thin film circuit board substrate is loaded in a cleaning basket, and then the cleaning basket loaded with the thin film circuit board substrate is dipped in a cleaning agent.
In the invention, the material of the cleaning flower basket is preferably fluoroplastic or polypropylene.
In the invention, the temperature of the cleaning agent during cleaning is preferably 40-60 ℃, and more preferably 45-55 ℃.
In the invention, the film circuit board is immersed in the cleaning agent after the cleaning agent is heated to the temperature during cleaning.
In the present invention, the cleaning is preferably ultrasonic cleaning.
In the invention, the ultrasonic frequency of the ultrasonic cleaning is preferably 28-40 kHz, and more preferably 30-28 kHz.
In the invention, the ultrasonic power of the ultrasonic cleaning is preferably 100-300W, and more preferably 150-250W.
In the invention, the ultrasonic time of the ultrasonic cleaning is preferably 10-30 min, and more preferably 12.5-26 min.
The invention provides a preparation method of a thin film circuit board, which comprises the following steps:
cleaning and drying the thin film circuit board substrate according to the cleaning method of the technical scheme to obtain the cleaned thin film circuit board substrate;
and preparing a thin film circuit on the surface of the cleaned thin film circuit board substrate to obtain the thin film circuit board.
According to the invention, the thin film circuit board substrate is cleaned and dried according to the cleaning method of the technical scheme, so that the cleaned thin film circuit board substrate is obtained.
In the invention, after the cleaning, the film circuit board substrate is preferably dried after the residual cleaning agent on the surface is absorbed and dried. In the embodiment of the invention, nitrogen is preferably adopted to suck the residual cleaning agent on the surface of the cleaned film circuit board substrate. In the invention, the purity of the nitrogen is more than or equal to 99 percent.
In the invention, the drying temperature is preferably 120-200 ℃, and more preferably 135-180 ℃.
In the invention, the drying heat preservation time is preferably 2-4 h, and more preferably 2.5-3.5 h.
After the cleaned thin film circuit board substrate is obtained, the thin film circuit is prepared on the surface of the cleaned thin film circuit board substrate to obtain the thin film circuit board.
In the invention, the thin film circuit is prepared on the surface of the dried thin circuit substrate by adopting a physical vapor deposition, photoetching or etching method preferably to obtain the thin film circuit board.
In the present invention, the thin film circuit substrate is preferably a quartz substrate.
In order to further illustrate the present invention, the following detailed description of the technical solutions provided by the present invention is made with reference to the accompanying drawings and examples, but they should not be construed as limiting the scope of the present invention.
Example 1
According to 3 percent of ammonium fluoride and 8 percent of inorganic acid, wherein the inorganic acid comprises hydrofluoric acid and phosphoric acid, and the mass percentage of HF in the hydrofluoric acid is 38 wt%; h in the phosphoric acid 3 PO 4 The mass percentage content of the component (A) is 85 wt%; the volume percentage content of hydrofluoric acid in the inorganic acid is 15%, the hydrogen peroxide is 6%, the ethanol is 15%, the sodium stearyl sulfate is 0.5%, and the balance of water are proportioned, and then the components are uniformly mixed to obtain the cleaning agent.
Example 2
According to 3% of ammonium fluoride and 8% of inorganic acid, wherein the inorganic acid comprises hydrofluoric acid and phosphoric acid, and the mass percentage of HF in the hydrofluoric acid is 40 wt%; h in the phosphoric acid 3 PO 4 The mass percentage content of (B) is 82 wt%; the volume percentage content of hydrofluoric acid in the inorganic acid is 15%, the hydrogen peroxide is 6%, the ethanol is 15%, the sodium stearate is 0.5%, and the balance of water are proportioned, and then the components are uniformly mixed to obtain the cleaning agent.
Example 3
According to 4 percent of ammonium fluoride and 6 percent of inorganic acid, wherein the inorganic acid comprises hydrofluoric acid and phosphoric acid, and the mass percentage of HF in the hydrofluoric acid is 39 wt%; h in the phosphoric acid 3 PO 4 The mass percentage content of (A) is 84 wt%; the volume percentage content of hydrofluoric acid in the inorganic acid is 35%, the hydrogen peroxide is 8%, the ethanol is 12%, the sodium stearyl sulfate is 0.76%, and the balance of water are proportioned, and then the components are uniformly mixed to obtain the cleaning agent.
Example 4
According to 4 percent of ammonium fluoride and 6 percent of inorganic acid, wherein the inorganic acid is hydrofluoric acid and phosphoric acid, and the mass percentage of HF in the hydrofluoric acid is 38 wt%; h in the phosphoric acid 3 PO 4 The mass percentage content of (A) is 83 wt%; the hydrofluoric acid in the inorganic acid accounts for 35 percent by volume, the hydrogen peroxide accounts for 8 percent by volume, the ethanol accounts for 12 percent by volume, the sodium stearate accounts for 0.76 percent by volume, and the balance of water is mixed uniformly to obtain the cleaning agent.
Example 5
According to 1.5 percent of ammonium fluoride and 8 percent of inorganic acid, wherein the inorganic acid comprises hydrofluoric acid and phosphoric acid, and the mass percentage of HF in the hydrofluoric acid is 40 wt%; h in the phosphoric acid 3 PO 4 The mass percentage content of (A) is 84 wt%; the inorganic acid contains 40% of hydrofluoric acid by volume, 5% of hydrogen peroxide, 18% of ethanol, 0.8% of sodium stearate and the balance of water, and the components are uniformly mixed to obtain the cleaning agent.
Example 6
According to 1.5 percent of ammonium fluoride and 8 percent of inorganic acid, wherein the inorganic acid comprises hydrofluoric acid and phosphoric acid, and the mass percentage of HF in the hydrofluoric acid is 38.5 percent by weight; h in the phosphoric acid 3 PO 4 The mass percentage content of (A) is 83.5 wt%; the volume percentage content of hydrofluoric acid in the inorganic acid is 40%, the hydrogen peroxide is 5%, the ethanol is 18%, the sodium octadecyl sulfate is 0.8%, and the balance of water are proportioned, and then the components are uniformly mixed to obtain the cleaning agent.
Example 7
Loading a quartz substrate for processing the thin film circuit board in a cleaning flower basket, wherein the cleaning flower basket is made of fluoroplastic,
the cleaning agent prepared in the example 1 is injected into a glass container, the cleaning agent is heated to 60 ℃, a cleaning flower basket loaded with a quartz substrate is immersed into the cleaning agent, the quartz substrate is subjected to ultrasonic cleaning in ultrasonic cleaning equipment by the cleaning agent, the ultrasonic frequency of an ultrasonic cleaning machine is 30kHz, the ultrasonic power is 150W, the ultrasonic time is 20min, after the cleaning is finished, the quartz substrate is subjected to high-purity nitrogen gas suction to dry the cleaning agent remained on the surface, the drying is carried out for 3h at 150 ℃, a thin film circuit is processed on the cleaned and dried quartz substrate by a physical vapor deposition method, and the thin film circuit board is prepared.
Example 8
The quartz substrate for processing the thin film circuit board is loaded in a cleaning flower basket which is made of fluoroplastic,
the cleaning agent prepared in the example 1 is injected into a glass container, the cleaning agent is heated to 45 ℃, a cleaning flower basket loaded with a quartz substrate is immersed into the cleaning agent, the quartz substrate is subjected to ultrasonic cleaning in ultrasonic cleaning equipment, the ultrasonic frequency of an ultrasonic cleaning machine is 35kHz, the ultrasonic power is 200W, the ultrasonic time is 20min, after the cleaning is finished, the quartz substrate is subjected to high-purity nitrogen gas suction drying on the cleaning agent remained on the surface, the drying is carried out for 2h at 150 ℃, a thin film circuit is processed on the cleaned and dried quartz substrate by an etching method, and the thin film circuit board is prepared.
Example 9
Loading a quartz substrate for processing the thin film circuit board in a cleaning flower basket, wherein the cleaning flower basket is made of fluoroplastic,
the cleaning agent prepared in the example 1 is injected into a glass container, the cleaning agent is heated to 50 ℃, a cleaning flower basket loaded with a quartz substrate is immersed into the cleaning agent, the quartz substrate is subjected to ultrasonic cleaning in ultrasonic cleaning equipment by the cleaning agent, the ultrasonic frequency of an ultrasonic cleaning machine is 28kHz, the ultrasonic power is 250W, the ultrasonic time is 30min, after the cleaning is finished, the quartz substrate is subjected to high-purity nitrogen gas suction to dry the cleaning agent remained on the surface, the drying is carried out for 2h at the temperature of 200 ℃, a thin film circuit is processed on the cleaned and dried quartz substrate by a photoetching method, and the thin film circuit board is prepared.
Comparative example 1
Loading a quartz substrate for processing the thin film circuit board in a cleaning flower basket, wherein the cleaning flower basket is made of fluoroplastic,
injecting ethanol into a glass container, heating the ethanol to 60 ℃, immersing a cleaning flower basket loaded with a quartz substrate into the ethanol, ultrasonically cleaning the quartz substrate in ultrasonic cleaning equipment by using a cleaning agent, wherein the ultrasonic frequency of an ultrasonic cleaning machine is 30kHz, the ultrasonic power is 150W, and the ultrasonic time is 20min, after cleaning, sucking the residual cleaning agent on the surface of the quartz substrate by using high-purity nitrogen, drying for 3h at 150 ℃, processing a thin film circuit on the cleaned and dried quartz substrate by using a physical vapor deposition method, and preparing the thin film circuit board.
Comparative example 2
The quartz substrate for processing the thin film circuit board is loaded in a cleaning flower basket which is made of fluoroplastic,
injecting acetone into a glass container, heating ethanol to 45 ℃, immersing a cleaning flower basket loaded with a quartz substrate into the ethanol, ultrasonically cleaning the quartz substrate in ultrasonic cleaning equipment by using a cleaning agent, wherein the ultrasonic frequency of an ultrasonic cleaning machine is 30kHz, the ultrasonic power is 150W, and the ultrasonic time is 20min, after cleaning, sucking the residual cleaning agent on the surface of the quartz substrate by using high-purity nitrogen, drying for 3h at 150 ℃, processing a thin film circuit on the cleaned and dried quartz substrate by using a physical vapor deposition method, and preparing the thin film circuit board.
Comparative example 3
The preparation method of the cleaning agent is basically the same as that of the example 1, except that: the mass percentage of the ammonium fluoride is 0.5 percent;
a thin film circuit board was prepared according to example 7.
Comparative example 4
The preparation method of the cleaning agent is basically the same as that of the example 1, except that: the inorganic acid is only hydrofluoric acid;
a thin film circuit board was prepared according to example 7.
Comparative example 5
The preparation method of the cleaning agent is basically the same as that of the example 1, except that: the inorganic acid is only phosphoric acid;
a thin film circuit board was prepared according to example 7.
Comparative example 6
The preparation method of the cleaning agent is basically the same as that of the example 1, except that: the mass percentage of the inorganic acid is 2 percent;
a thin film circuit board was prepared according to example 7.
Comparative example 7
The preparation method of the cleaning agent is basically the same as that of the example 1, except that: the mass percentage content of the hydrogen peroxide is 15 percent;
a thin film circuit board was prepared according to example 7.
Comparative example 8
The preparation method of the cleaning agent is basically the same as that of the example 1, except that: no surfactant is added;
a thin film circuit board was prepared according to example 7.
Test example
The performance test of the quartz substrate thin film circuit board processed in example 7 of the present invention and the quartz substrate thin film circuit board prepared in comparative example 1 was performed, and the test method was: gold wire bonding is carried out on the surface of the thin film circuit by using a gold wire with the diameter of 50 microns, a tensile force test is carried out on the bonded gold wire, the tensile force value is 45-60 grams force, the gold layer of the thin film circuit board prepared in the embodiment 7 of the invention is not peeled as shown in figure 1, the quartz thin film circuit (comparative example 1) processed by cleaning with conventional ethanol is used, gold wire bonding is carried out on the surface of the thin film circuit by using the gold wire with the diameter of 50 microns, the tensile force test is carried out on the bonded gold wire, the tensile force value is 25-40 grams force, and the gold layer is peeled as shown in figure 2.
The test results of the quartz substrate thin film circuit boards processed in examples 8 and 9 were similar to those of example 7.
The test effect of the cleaning agent prepared in the embodiment 2-9 on the quartz substrate thin film circuit board processed by the processing method provided in the embodiment 7 is similar to the test result of the embodiment 7.
Comparative example 2 the test results of the quartz substrate thin film circuit board processed were similar to those of example 7.
The test results of the quartz substrate thin film circuit boards processed in comparative examples 3 to 8 are higher in binding force than the test results of the quartz substrate thin film circuit boards processed in comparative examples 1 and 2, but lower in binding force than the quartz substrate thin film circuit board processed in example 7.
In conclusion, the invention provides a cleaning agent, which comprises the following components in percentage by mass: 1-5% of ammonium fluoride, 3-10% of inorganic acid, 5-10% of hydrogen peroxide, 10-20% of ethanol, 0.1-1% of surfactant and the balance of water; the inorganic acid comprises hydrofluoric acid and/or phosphoric acid; the mass percentage of HF in the hydrofluoric acid is 38-40 wt%; h in the phosphoric acid 3 PO 4 The content of (b) is 82-85 wt%. The cleaning agent provided by the invention is prepared by compounding ammonium fluoride, hydrofluoric acid and/or phosphoric acid, hydrogen peroxide, ethanol, a surfactant and water, and simultaneously regulating and controlling the cleaning agent obtained by the raw materials in the range, compared with the conventional acidic cleaning agent, alkaline cleaning agent or organic solvent cleaning agent such as acetone, ethanol and the like, the cleaning agent can effectively remove pollutants attached to the surface of a quartz substrate, so that the adhesive force of the methods such as physical vapor deposition, photoetching or etching and the like in the process of preparing a metal film on the surface of the quartz substrate is improved, and the finally processed film circuit board effectively avoids the phenomenon that the metal film falls off from the surface of the quartz substrate
Although the present invention has been described in detail with reference to the above embodiments, it is only a part of the embodiments of the present invention, not all of the embodiments, and other embodiments can be obtained without inventive step according to the embodiments, and all of the embodiments belong to the protection scope of the present invention.
Claims (10)
1. The cleaning agent is characterized by comprising the following components in percentage by mass:
1-5% of ammonium fluoride, 3-10% of inorganic acid, 5-10% of hydrogen peroxide, 10-20% of ethanol, 0.1-1% of surfactant and the balance of water; the inorganic acid comprises hydrofluoric acid and/or phosphoric acid; the mass percentage of HF in the hydrofluoric acid is 38-40 wt%;h in the phosphoric acid 3 PO 4 The mass percentage of the component (A) is 82-85 wt%.
2. The cleaning agent according to claim 1, wherein the inorganic acid comprises hydrofluoric acid and phosphoric acid, and the volume percentage of the hydrofluoric acid in the inorganic acid is 10-50%.
3. The cleaning formulation defined in claim 1, wherein the surfactant comprises sodium stearyl sulfate and/or sodium stearate.
4. The use of the cleaning agent according to any one of claims 1 to 3 for cleaning a thin film circuit board substrate.
5. A method for cleaning a thin film circuit board substrate is characterized by comprising the following steps:
the film circuit board substrate is soaked in a cleaning agent for cleaning, wherein the cleaning agent is the cleaning agent as defined in any one of claims 1-3.
6. The cleaning method according to claim 5, wherein the temperature of the cleaning agent is 40 to 60 ℃ during the cleaning.
7. The cleaning method according to claim 5 or 6, wherein the cleaning is ultrasonic cleaning, the ultrasonic frequency of the ultrasonic cleaning is 28-40 kHz, and the ultrasonic power of the ultrasonic cleaning is 100-300W.
8. The cleaning method according to claim 7, wherein the ultrasonic time of the ultrasonic cleaning is 10 to 30 min.
9. The preparation method of the thin film circuit board is characterized by comprising the following steps:
cleaning and drying the thin film circuit board substrate according to the cleaning method of any one of claims 5 to 8 to obtain a cleaned thin film circuit board substrate;
and preparing a thin film circuit on the surface of the cleaned thin film circuit board substrate to obtain the thin film circuit board.
10. The preparation method according to claim 9, wherein the drying temperature is 120 to 200 ℃, and the drying holding time is 2 to 4 hours.
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| CN1144399A (en) * | 1995-03-27 | 1997-03-05 | 索尼公司 | Method of cleaning substrate |
| CN1828841A (en) * | 2005-02-23 | 2006-09-06 | 东京毅力科创株式会社 | Method of surface processing substrate, method of cleaning substrate, and programs for implementing the methods |
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