CN112375570A - Etching solution for etching through hole or depression on substrate and preparation method and application thereof - Google Patents

Etching solution for etching through hole or depression on substrate and preparation method and application thereof Download PDF

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CN112375570A
CN112375570A CN202011240814.4A CN202011240814A CN112375570A CN 112375570 A CN112375570 A CN 112375570A CN 202011240814 A CN202011240814 A CN 202011240814A CN 112375570 A CN112375570 A CN 112375570A
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etching
etching solution
substrate
alcohol
solution
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CN112375570B (en
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张轶鸣
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Taijiwei Technology Suzhou Co ltd
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Taijiwei Technology Wuxi Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K13/00—Etching, surface-brightening or pickling compositions
    • C09K13/02—Etching, surface-brightening or pickling compositions containing an alkali metal hydroxide
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C15/00—Surface treatment of glass, not in the form of fibres or filaments, by etching
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
    • H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
    • H01L21/30604—Chemical etching

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
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  • Manufacturing & Machinery (AREA)
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  • Geochemistry & Mineralogy (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Physics & Mathematics (AREA)
  • Surface Treatment Of Glass (AREA)

Abstract

The invention relates to an etching solution for etching through holes or depressions on a substrate, a preparation method and application thereof, wherein the etching solution comprises alkali, alcohol and solvent water; the content of alkali in the etching solution is 20-50% by mass; the alcohol in the etching solution accounts for 5-20% by volume fraction. The etching solution provided by the invention realizes high-efficiency etching of a specific area of a substrate by introducing the specific alcohol component, and avoids the problem of over-etching caused by hydrofluoric acid etching solution. The introduction of the alcohol reduces the surface tension of the etching solution, so that the etching solution can more easily penetrate into the microstructure on the surface of the glass, and the etching is accelerated.

Description

Etching solution for etching through hole or depression on substrate and preparation method and application thereof
Technical Field
The invention relates to the field of basic etching, in particular to etching solution for through hole or recess etching on a substrate and a preparation method and application thereof.
Background
At present, the introduction of vias or recesses on substrates used as interposers or microcomponents is generally carried out by a process of masking + hydrofluoric acid chemical etching or laser irradiation + hydrofluoric acid chemical etching.
For example, CN105102177A discloses a method and a device for introducing a plurality of recesses (5) in a substrate (2) used as an interposer by means of a laser beam, and a substrate (2) manufactured in this way. For this purpose, a laser beam (3) is directed onto the surface of the substrate (2). In this case, the duration of action of the laser beam (3) is selected to be very short, so that only a modification of the substrate (2) concentrically around the optical axis (Z) of the laser beam occurs, without removal of substrate material. Firstly, a laser beam (3) is guided through a transmission medium (8) having a refractive index that is greater than air and depends on the intensity; the laser beam (3) then reaches the substrate (2). The refractive index also changes because the intensity of the pulsed laser used is not constant but has an intensity that rises to a maximum and then falls within a single pulse length. Thereby, the focal point (9a) of the laser beam (3) is displaced along the optical axis (Z) between the outer surfaces (11,12) of the substrate (2), thereby obtaining the desired modification along the optical axis (Z) without having to trace the laser processing head (10) on the optical axis (Z).
CN107540232A discloses a glass processing method, which comprises a step of forming a through hole (11) on a glass substrate (10) by laser; and a step of wet etching the through-hole (11) with an etching solution (34). The etching liquid (34) contains hydrofluoric acid and a first liquid, and the first liquid is formed of an acid having a molecular size larger than that of the hydrofluoric acid. The concentration of hydrofluoric acid is 4 wt% or less. The concentration of the first liquid is higher than the concentration of hydrofluoric acid.
However, hydrofluoric acid has strong corrosivity and volatility, and the glass etching process using hydrofluoric acid has high requirements on sealing and ventilation of an etching environment, and further, the hydrofluoric acid has the problem of over-etching in the use process.
Disclosure of Invention
In view of the problems in the prior art, the present invention aims to provide an etching solution for etching through holes or pits on a substrate, a preparation method and a use thereof, which realizes efficient etching of a specific region of the substrate by adopting specific components through redesigning the etching solution, and avoids the over-etching problem caused by hydrofluoric acid based etching solutions.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides an etching solution for etching through holes or depressions on a substrate, which comprises alkali, alcohol and solvent water;
the content of alkali in the etching solution is 20-50% by mass;
the alcohol in the etching solution accounts for 5-20% by volume fraction.
The etching solution provided by the invention realizes high-efficiency etching of a specific area of a substrate by introducing the specific alcohol component, and avoids the problem of over-etching caused by hydrofluoric acid etching solution. The introduction of the alcohol reduces the surface tension of the etching solution, so that the etching solution can more easily penetrate into the microstructure on the surface of the glass, and the etching is accelerated.
In the present invention, the amount of the base in the etching solution is 20 to 50% by mass, and may be, for example, 20%, 21%, 22%, 23%, 24%, 25%, 26%, 27%, 28%, 29%, 30%, 31%, 32%, 33%, 34%, 35%, 36%, 37%, 38%, 39%, 40%, 41%, 42%, 43%, 44%, 45%, 46%, 47%, 48%, 49%, or 50%, but is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable.
In the present invention, the alcohol in the etching solution may be 5 to 20% by volume, for example, 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19%, or 20%, but is not limited to the above-mentioned values, and other values not listed in the above range are also applicable.
As a preferred embodiment of the present invention, the alkali includes sodium hydroxide and/or potassium hydroxide.
Preferably, the alcohol comprises a combination of 1 or at least 2 of methanol, ethanol or isopropanol, which may be a combination of methanol and ethanol, ethanol and isopropanol or methanol and isopropanol, and the like, but is not limited to the listed combinations, and other combinations not listed within this range are equally suitable.
Preferably, the pH of the etching solution is 11 or more, for example, 11, 11.2, 11.4, 11.6, 11.8, 12, 12.2, 12.4, 12.6, 12.8, 13, 13.2, 13.4, 13.6, 13.8 or 14, but is not limited to the values listed, and other values not listed in this range are also applicable.
In the invention, due to the existence of hydrogen bonds in the primary aqueous solution, the solution has large viscosity and poor fluidity, the internal alkali component is slowly diffused, and the introduction of alcohol can effectively destroy the hydrogen bonds in the primary aqueous solution, reduce the solution viscosity and improve the diffusion rate of the alkali component. Since the chemical reaction rate is proportional to the mass exchange rate, the introduction of alcohol can accelerate the etching reaction.
In a second aspect, the present invention provides a method for preparing the etching solution according to the first aspect, the method comprising: and mixing the alkali solution and the alcohol according to the proportion to obtain the etching solution.
In a third aspect, the present invention provides a use of the etching solution according to the first aspect, the use comprising the steps of:
(1) processing the substrate by using laser or rays to obtain an intermediate substrate;
(2) and (3) placing the intermediate substrate obtained in the step (1) in an etching solution for etching to obtain a substrate with through holes or depressions.
In the present invention, the radiation is high-energy radiation, and may be, for example, arc discharge.
In a preferred embodiment of the present invention, the substrate in step (1) is made of silicon and/or silicate, preferably glass.
The glass in the present invention may be ordinary glass, quartz glass, boron glass, or the like.
As a preferable embodiment of the present invention, the treatment in the step (2) is irradiation treatment of a via region or a recess region of the substrate into which the via hole or the recess is to be introduced.
As a preferable technical scheme of the invention, the etching in the step (2) is carried out under ultrasonic conditions.
As a preferred embodiment of the present invention, the frequency of the ultrasound in the etching in the step (2) is > 28kHz, and may be, for example, 29kHz, 29.2kHz, 29.4kHz, 29.6kHz, 29.8kHz, 30kHz, 30.2kHz, 30.4kHz, 30.6kHz, 30.8kHz, 31kHz, 31.2kHz, 31.4kHz, 31.6kHz, 31.8kHz, 32kHz, 32.2kHz, 32.4kHz, 32.6kHz, 32.8kHz, 33kHz, 34kHz or 35kHz, etc., but is not limited to the above-mentioned values, and other values not mentioned in this range are also applicable.
In a preferred embodiment of the present invention, the time of the ultrasonic treatment in the etching in the step (2) is more than 0.5h, for example, 0.6h, 0.7h, 0.8h, 0.9h, 1h, 1.2h, 1.4h, 1.6h, 1.8h or 2h, but is not limited to the above-mentioned values, and other values not listed in the above range are also applicable.
As a preferred technical scheme of the invention, the application comprises the following steps:
(1) processing the glass substrate by using laser or rays to obtain an intermediate substrate;
(2) placing the intermediate substrate in the step (1) in an etching solution for etching to obtain a substrate with through holes or depressions;
the etching is carried out under ultrasonic conditions, the frequency of the ultrasonic is more than 28kHz, and the time is more than 0.5 h.
Compared with the prior art, the invention at least has the following beneficial effects:
(1) the etching solution provided by the invention realizes high-efficiency etching of a specific area of a substrate by introducing the specific alcohol component, and avoids the problem of over-etching caused by hydrofluoric acid etching solution.
(2) The introduction of the alcohol reduces the surface tension of the etching solution, so that the etching solution can more easily penetrate into the microstructure on the surface of the glass, the etching is strengthened, and furthermore, the addition of the alcohol can promote the material exchange between the etching solution and the substrate and accelerate the etching reaction.
Detailed Description
To better illustrate the invention and to facilitate the understanding of the technical solutions thereof, typical but non-limiting examples of the invention are as follows:
example 1
The embodiment provides an etching solution for etching through holes or pits on a substrate, wherein the etching solution comprises alkali, alcohol and solvent water;
the sodium hydroxide in the etching solution accounts for 35% by mass;
the volume fraction of ethanol in the etching solution is 13%.
The preparation method comprises the following steps:
and mixing the sodium hydroxide solution and the ethanol according to the proportion to obtain the etching solution.
Example 2
The embodiment provides an etching solution for etching through holes or pits on a substrate, wherein the etching solution comprises alkali, alcohol and solvent water;
the sodium hydroxide in the etching solution accounts for 20% by mass;
the volume fraction of ethanol in the etching solution is 18%.
The preparation method comprises the following steps:
and mixing the sodium hydroxide solution and the ethanol according to the proportion to obtain the etching solution.
Example 3
The embodiment provides an etching solution for etching through holes or pits on a substrate, wherein the etching solution comprises alkali, alcohol and solvent water;
the sodium hydroxide in the etching solution accounts for 47 percent by mass;
the volume fraction of ethanol in the etching solution is 7%.
The preparation method comprises the following steps:
and mixing the sodium hydroxide solution and the ethanol according to the proportion to obtain the etching solution.
Application example 1
The present application example provides use of the etching solution provided in example 1, the use including the steps of:
(1) processing the glass substrate by using laser to obtain an intermediate substrate;
(2) and (3) placing the intermediate substrate obtained in the step (1) in an etching solution for etching to obtain a substrate with a through hole.
The treatment is to irradiate the through hole area of the substrate to be introduced into the through hole;
the etching was carried out under ultrasonic conditions with a frequency of 29kHz and a time of 0.6 h.
Application example 2
The present application example provides use of the etching solution provided in example 1, the use including the steps of:
(1) processing the glass substrate by using arc discharge to obtain an intermediate substrate;
(2) and (3) placing the intermediate substrate obtained in the step (1) in an etching solution for etching to obtain a substrate with a recess.
The treatment is to perform irradiation treatment on a substrate concave area to be introduced with a concave;
the etching was carried out under ultrasonic conditions with a frequency of 29kHz and a time of 1 h.
Application example 3
The present application example provides use of the etching solution provided in embodiment 2, the use including the steps of:
(1) processing a silicon substrate by using laser to obtain an intermediate substrate;
(2) and (3) placing the intermediate substrate obtained in the step (1) in an etching solution for etching to obtain a substrate with a through hole.
The treatment is to irradiate the through hole area of the substrate to be introduced into the through hole;
the etching was carried out under ultrasonic conditions with a frequency of 30kHz and a time of 0.7 h.
Application example 4
The present application example provides use of the etching solution provided in embodiment 2, the use including the steps of:
(1) processing the sapphire substrate by using arc discharge to obtain an intermediate substrate;
(2) and (3) placing the intermediate substrate obtained in the step (1) in an etching solution for etching to obtain a substrate with a recess.
The treatment is to perform irradiation treatment on a sunken area of the substrate into which the sunken part is to be introduced;
the etching was carried out under ultrasonic conditions with a frequency of 31kHz and a time of 0.8 h.
Application example 5
The present application example provides use of the etching solution provided in example 3, the use including the steps of:
(1) processing the glass substrate by using laser to obtain an intermediate substrate;
(2) and (3) placing the intermediate substrate obtained in the step (1) in an etching solution for etching to obtain a substrate with a through hole.
The treatment is to irradiate the through hole area of the substrate to be introduced into the through hole;
the etching is carried out under ultrasonic conditions, the frequency of the ultrasonic is 35kHz, and the time is 1 h.
Application example 6
The present application example provides use of the etching solution provided in example 3, the use including the steps of:
(1) processing the glass substrate by using laser to obtain an intermediate substrate;
(2) and (3) placing the intermediate substrate obtained in the step (1) in an etching solution for etching to obtain a substrate with a recess.
The treatment is to perform irradiation treatment on a sunken area of the substrate into which the sunken part is to be introduced;
the etching was carried out under ultrasonic conditions with a frequency of 35kHz and a time of 0.6 h.
Comparative example 1
The difference from the embodiment 1 is only that the mass percentage of the sodium hydroxide in the etching solution is 60%, the etching solution is over-etched in some positions, and is under-etched in some positions, which is a non-uniform phenomenon, the etching surface is rough, and for the groove or hole with the depth-to-diameter ratio exceeding 10, the condition of internal under-etching is easy to occur, and an inverted cone-shaped cross section structure is formed.
Comparative example 2
The difference from the embodiment 1 is only that the mass percentage of the sodium hydroxide in the etching solution is 10 percent, the etching speed is obviously reduced,
comparative example 3
The difference from the embodiment 1 is only that the volume fraction of ethanol in the etching solution is 2%, the amount of ethanol lack is complemented with water, the mass percentage content of sodium hydroxide is ensured to be unchanged, and the reaction rate is obviously reduced.
Comparative example 4
The difference from the embodiment 1 is only that the volume fraction of ethanol in the etching solution is 35%, the amount of ethanol is increased, the amount of water is adaptively reduced, the mass percentage of sodium hydroxide is kept unchanged, the proportion of alcohol is increased, the alkali concentration in equivalent water is increased, the etching reaction is easy to have uneven etching, namely, the alcohol content in the etching solution is closely related to the concentration of sodium hydroxide, and strict matching is needed.
Comparative example 5
The difference from the embodiment 1 is only that the ethanol in the etching solution is converted into the mass content and is replaced by the sodium gluconate, the viscosity of the solvent is further increased compared with the solvent without increasing the alcohol solvent, and the inside underetching condition is easy to occur in the groove or the hole with the depth-diameter ratio exceeding 10, so that the inverted cone-shaped cross-section structure is formed.
As can be seen from the results of the above examples and comparative examples, the etching solution provided by the present invention realizes efficient etching of a specific region of a substrate by introducing a specific alcohol component, and avoids the problem of over-etching caused by a hydrofluoric acid-based etching solution. The introduction of the alcohol reduces the surface tension of the etching solution, so that the etching solution can more easily penetrate into the microstructure on the surface of the glass, and the addition of the alcohol can promote the exchange of substances between the etching solution and the substrate and accelerate the etching reaction.
The applicant declares that the present invention illustrates the detailed structural features of the present invention through the above embodiments, but the present invention is not limited to the above detailed structural features, that is, it does not mean that the present invention must be implemented depending on the above detailed structural features. It should be understood by those skilled in the art that any modifications of the present invention, equivalent substitutions of selected components of the present invention, additions of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.

Claims (10)

1. The etching solution for etching the through hole or the depression on the substrate is characterized by comprising alkali, alcohol and solvent water;
the content of alkali in the etching solution is 20-50% by mass;
the alcohol in the etching solution accounts for 5-20% by volume fraction.
2. The etching solution of claim 1, wherein the base comprises sodium hydroxide and/or potassium hydroxide;
preferably, the alcohol comprises 1 or a combination of at least 2 of methanol, ethanol or isopropanol;
preferably, the pH value of the etching solution is more than or equal to 11.
3. The method of preparing an etching solution according to claim 1 or 2, comprising: and mixing the alkali solution and the alcohol according to the proportion to obtain the etching solution.
4. Use of an etching solution according to claim 1 or 2, characterized in that it comprises the following steps:
(1) processing the substrate by using laser or rays to obtain an intermediate substrate;
(2) and (3) placing the intermediate substrate obtained in the step (1) in an etching solution for etching to obtain a substrate with through holes or depressions.
5. Use according to claim 4, wherein the substrate of step (1) is made of silicon and/or silicate, preferably glass, as the main material.
6. The use according to claim 4 or 5, wherein the treatment of step (2) is an irradiation treatment of a via region or a recess region of the substrate to be introduced with a via hole or recess.
7. Use according to any one of claims 4 to 6, wherein the etching of step (2) is carried out under ultrasonic conditions.
8. Use according to any one of claims 4 to 7, wherein the frequency of ultrasound in the etching of step (2) is > 28 kHz.
9. Use according to any one of claims 4 to 8, wherein the time of sonication in the etching of step (2) is > 0.5 h.
10. Use according to any one of claims 4 to 9, characterized in that it comprises the following steps:
(1) processing the glass substrate by using laser or rays to obtain an intermediate substrate;
(2) placing the intermediate substrate in the step (1) in an etching solution for etching to obtain a substrate with through holes or depressions;
the etching is carried out under ultrasonic conditions, the frequency of the ultrasonic is more than 28kHz, and the time is more than 0.5 h.
CN202011240814.4A 2020-11-09 2020-11-09 Etching solution for etching through hole or depression on substrate and preparation method and application thereof Active CN112375570B (en)

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CN113045209A (en) * 2021-03-02 2021-06-29 广东芯华微电子技术有限公司 Glass through hole machining method
CN113860753A (en) * 2021-09-29 2021-12-31 维达力实业（赤壁）有限公司 Glass hole opening method
CN114455858A (en) * 2022-01-27 2022-05-10 醴陵旗滨电子玻璃有限公司 Glass strengthening method, glass substrate, and etching material for glass

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CN113045209A (en) * 2021-03-02 2021-06-29 广东芯华微电子技术有限公司 Glass through hole machining method
CN113860753A (en) * 2021-09-29 2021-12-31 维达力实业（赤壁）有限公司 Glass hole opening method
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CN114455858B (en) * 2022-01-27 2024-02-27 湖南旗滨电子玻璃股份有限公司 Glass strengthening method, glass substrate and etching material for glass

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