CN111499915A - Surface treatment method of L CP film - Google Patents
Surface treatment method of L CP film Download PDFInfo
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- CN111499915A CN111499915A CN201911390926.5A CN201911390926A CN111499915A CN 111499915 A CN111499915 A CN 111499915A CN 201911390926 A CN201911390926 A CN 201911390926A CN 111499915 A CN111499915 A CN 111499915A
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- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/02—Chemical treatment or coating of shaped articles made of macromolecular substances with solvents, e.g. swelling agents
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/12—Chemical modification
- C08J7/14—Chemical modification with acids, their salts or anhydrides
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Abstract
The invention provides a surface treatment method of an L CP film, which fills the blank of the surface treatment method of a L CP film in the prior art, and has the advantages of conventional chemical treatment method, simple operation, low threshold, cheap and easily-obtained production condition equipment and raw materials, and easy realization and popularization.
Description
[ technical field ] A method for producing a semiconductor device
The invention relates to the field of material surface treatment, in particular to a surface treatment method of an L CP film.
[ background of the invention ]
In recent years, with the rapid development of the electronic industry, the basic material of Printed Circuit Board (PCB for short) plays a key role in connecting and supporting electronic components, and the copper clad laminate (CC L) is the basic material of the Circuit Board, so that the Printed Circuit Board has wide application in many electronic products.
According to the difference of base materials in the copper clad laminate, the copper clad laminate can be generally divided into a rigid copper clad laminate which is not easy to bend and a bendable flexible copper clad laminate, wherein the bendable flexible copper clad laminate has the outstanding advantage of reducing the volume and the weight of equipment.
Wearable in people's daily life, portable smart machine has become indispensable necessities such as smart mobile phone, wrist-watch, panel computer to more and more pursuing short and small frivolous, multi-functional, signal transmission high speed to these equipment, under the circumstances that these applications are developing rapidly, will be to the demand of flexible copper-clad plate bigger and bigger.
Polyimide (PI), Polyester (PET), Polynaphthalene Ester (PEN) and the like are mainly used in flexible radio frequency antenna circuit board materials in the market at present, the PET and the PEN are poor in heat resistance and high in PI water absorption rate, the defects can cause curling of a substrate film and reduction of peeling strength of a copper foil, and simultaneously, dielectric properties can be reduced, and transmission of electric signals is influenced finally.
The liquid crystal polymer (L CP) material is used as a thermoplastic resin, has the characteristics of good mechanical property and heat resistance, high dimensional stability, low thermal expansion coefficient, low dielectric constant, loss and the like, can completely avoid the defects of the materials, and particularly has great application in fifth-generation communication equipment.
The copper-clad method of the thermoplastic liquid crystal polymer flexible copper-clad plate mainly comprises the steps of controlling the temperature between the thermal deformation temperature and the melting point of a liquid crystal polymer, pressing the liquid crystal polymer and a copper foil, and cooling the liquid crystal polymer flexible copper-clad plate, wherein the control on the temperature and the pressure in the pressing process is particularly critical, the control determines the thickness uniformity and the peel strength of the produced copper-clad plate, so that whether the copper-clad plate is qualified or not is influenced, and when the peel strength is not high, in order to realize good combination, the surface of an L CP film can be modified, so that the combination force between the two is improved.
The prior art has no mature L CP film surface treatment method.
Therefore, it is necessary to provide a surface treatment method of L CP film suitable for industrial application.
[ summary of the invention ]
The invention aims to provide an L CP film surface treatment method to make up the blank of the prior art in the aspect of L CP film surface treatment.
In order to solve the above problems, the present invention provides a surface treatment method of L CP film, comprising the following steps:
heating and swelling the L CP film in an alcohol ether solution containing strong base, wherein the content of the strong base in the alcohol ether solution containing the strong base is 1-20 g/L, the content of ethers is 1-18 g/L, and the content of alcohols is 0.1-1.5 g/L;
etching the swollen L CP film in a first mixed solution formed by strong base and strong oxidant, wherein the solvent in the first mixed solution is water, the content of the strong base is 1-20 g/L, and the content of the strong oxidant is 4-30 g/L;
reducing the L CP film subjected to etching treatment in a second mixed solution formed by strong acid and oxalate, wherein the content of the strong acid in the second mixed solution is 10-50 ml/L, and the content of the oxalate in the second mixed solution is 3-18 g/L;
the reduced L CP film was washed and dried.
Preferably, the strong base is at least one of potassium hydroxide, sodium hydroxide and lithium hydroxide.
Preferably, the solvent of the alcohol ether solution is at least one of ethylene glycol methyl ether, ethylene glycol ethyl ether, ethylene glycol, propylene glycol and hexylene glycol.
Preferably, the strong oxidant is at least one of potassium manganate, potassium permanganate and potassium dichromate.
Preferably, the strong acid is at least one of hydrochloric acid, nitric acid and concentrated sulfuric acid.
Preferably, the oxalate is at least one of ammonium oxalate, sodium oxalate and potassium oxalate.
Preferably, the temperature of the heating swelling treatment is 40-90 ℃, and the treatment time is 3-30 min.
Preferably, the processing temperature of the etching treatment is 40-90 ℃, and the processing time is 10-120 min.
Preferably, the temperature of the reduction treatment is 10-50 ℃, and the treatment time is 1-10 min.
Preferably, the temperature of the drying treatment is 100-200 ℃, and the time is 30-120 min. .
Compared with the prior art, firstly, the L CP film with a relatively smooth surface is coarsened to obtain the copper-clad plate with good bonding force, so that the blank of the surface treatment method of the L CP film is made up, and in addition, the adopted chemical treatment method is conventional, the operation is simple, the threshold is low, the production condition, equipment and raw materials are cheap and easy to obtain, and the copper-clad plate is easy to realize and popularize.
[ description of the drawings ]
FIG. 1 is an SEM image and a surface roughness characterization image of L CP thin film and original film after surface treatment according to example 1 of the present invention;
FIG. 2 is a graph showing the peel force of treated L CP film and copper foil after thermoforming in accordance with example 1 of the present invention;
FIG. 3 is an SEM image and a surface roughness characterization of L CP film and original film after surface treatment according to example 2 of the present invention;
FIG. 4 is a graph showing the peel force of treated L CP film and copper foil after thermoforming in accordance with example 2 of the present invention;
FIG. 5 is an SEM image and a surface roughness characterization of L CP film and original film after surface treatment according to example 3 of the present invention;
fig. 6 is a graph showing the peel force test of the treated L CP film and copper foil after thermoforming in example 3 of the present invention.
[ detailed description ] embodiments
The embodiment of the invention provides a surface treatment method of an L CP film, which comprises the following steps:
s01, heating and swelling the L CP film in an alcohol ether solution containing strong base, wherein the content of the strong base in the alcohol ether solution containing the strong base is 1-20 g/L, the content of ethers is 1-18 g/L, and the content of alcohols is 0.1-1.5 g/L;
s02, etching the swollen L CP film in a first mixed solution formed by strong alkali and a strong oxidant, wherein the solvent in the first mixed solution is water, the content of the strong alkali is 1-20 g/L, and the content of the strong oxidant is 4-30 g/L;
s03, reducing the etched L CP film in a second mixed solution formed by strong acid and oxalate, wherein the content of the strong acid in the second mixed solution is 10-50 ml/L, and the content of the oxalate is 3-18 g/L;
s04, washing and drying the L CP film subjected to the reduction treatment.
In practical production, the L CP film inevitably has oil stains after being produced, so that the oil stains need to be removed by ultrasonic cleaning, and the ultrasonic treatment is usually carried out for 10-60min by adopting an environment-friendly and recyclable organic solvent, so that the reduction of the processing quality and efficiency caused by the pollution of the oil stains to the next processing liquid is avoided.
In the above step S01, the strong base is at least one of potassium hydroxide, sodium hydroxide, and lithium hydroxide. The alkali metal hydroxide is selected as the strong alkali, the reason is that the subsequent steps comprise neutralization and cleaning of alkali, the salt formed after the alkali metal neutralization has the best solubility and is easy to clean, and other strong alkali can cause the problems of difficult and incomplete cleaning and the like.
In the step S01, the solvent of the alcohol ether solution is at least one of ethylene glycol methyl ether, ethylene glycol ethyl ether, ethylene glycol, propylene glycol, and hexylene glycol. The alcohol and strong alkali can be used to form sodium alkoxide, potassium alkoxide and lithium alkoxide which have stronger basicity than alkali metal hydroxide, so as to enhance the chemical swelling effect.
In the step S01, the temperature of the heating swelling treatment is 40-90 ℃, and the treatment time is 3-30 min. The temperature can be reasonably selected according to the boiling point of the solvent, and the treatment time can be reasonably selected according to the swelling effect achieved by different solvents.
In step S02, the strong oxidant is at least one of potassium manganate, potassium permanganate, and potassium dichromate. These are salts of strong oxidants, have good solubility, and can have good etching effect by matching with strong alkali.
In the step S02, the etching temperature is 40-90 ℃, and the etching time is 10-120 min. The temperature and time are also reasonably controlled according to the choice of the solvent and different oxidants.
In the step S03, the strong acid is at least one of hydrochloric acid, nitric acid, and concentrated sulfuric acid. The acid selected here is three strong acids, which can provide a suitable pH to facilitate the reduction of the residual oxidant by oxalic acid. In addition, the residual strong base can be neutralized.
In step S03, the oxalate is at least one of ammonium oxalate, sodium oxalate, and potassium oxalate. Oxalic acid is oxidized by a strong oxidant to become carbon dioxide which is easy to remove, so oxalate ions are selected as a reducing agent, and in addition, selected ammonium ions, sodium ions and potassium ions are also easy to dissolve or can be directly removed.
In the step S03, the temperature of the reduction treatment is 10-50 ℃, and the treatment time is 1-10 min. Because the reaction between oxalic acid and the strong oxidant is very rapid, the lower temperature needs to be properly controlled, and the over-violent reaction is avoided.
In the step S04, the temperature of the drying treatment is 100-.
The invention is further described with reference to the following figures and detailed description.
Example 1
The L CP film surface processing method of the embodiment comprises the following steps:
removing oil from L CP film by ultrasonic treatment in ethanol for 10 min;
swelling the L CP film subjected to oil removal treatment in strong alkali alcohol ether solution at 40 ℃ for 30min, wherein the contents of sodium hydroxide, ethylene glycol monomethyl ether, hexanediol and water in the solution are respectively 1g, 1.4g, 0.1g and 1L;
etching the swollen L CP film in a mixed solution of sodium hydroxide and potassium permanganate at 40 ℃ for 120min, wherein the sodium hydroxide, the potassium permanganate and the water in the mixed solution are respectively 1g, 4g and 1L;
reducing the L CP film subjected to etching treatment in a mixed solution of sulfuric acid and sodium oxalate at 50 ℃ for 1min, wherein the sulfuric acid, the sodium oxalate and water in the mixed solution are respectively 10ml, 3g and 1L;
the reduced L CP film was washed and dried in an oven at 200 deg.C for 30min to give a treated L CP film.
The microstructure of the L CP film surface obtained in the example was changed from the original film (FIG. 1A) surface and the surface roughness (FIG. 1D) was increased from 0.172 μm to 0.282 μm as shown in FIG. 1B, and the L CP film obtained in the example was significantly improved by the peel force of 0.63N/mm measured by the hot-pressing treatment of the original film (FIG. 1C) with a copper foil having a surface roughness of 0.706 μm as shown in FIG. 2, compared to 0.54N/mm measured after the same hot-pressing treatment of the untreated L CP film with the same copper foil.
Example 2
The L CP film surface processing method of the embodiment comprises the following steps:
ultrasonically treating L CP film in ethanol for 30min to remove oil;
swelling the L CP film subjected to oil removal treatment in strong alkali alcohol ether solution at 75 ℃ for 15min, wherein the sodium hydroxide, ethylene glycol monomethyl ether, hexanediol and water in the solution are respectively 12g, 13g, 1g and 1L;
etching the swollen L CP film in a mixed solution of sodium hydroxide and potassium permanganate at 75 ℃ for 60min, wherein the sodium hydroxide, the potassium permanganate and the water in the mixed solution are respectively 10g, 20g and 1L;
reducing the L CP film subjected to etching treatment in a mixed solution of sulfuric acid and sodium oxalate at 30 ℃ for 5min, wherein the sulfuric acid, the sodium oxalate and water in the mixed solution are respectively 24ml, 8g and 1L;
the reduced L CP film was washed and dried in an oven at 160 deg.C for 90min to give a treated L CP film.
The microstructure of the surface of the L CP film obtained in the example was changed from the surface of the original film (FIG. 3A) and the surface roughness (FIG. 3D) was increased from 0.172 μm to 0.523 μm as shown in FIG. 3B, the peel force of the L CP film obtained in the example was 0.68N/mm as measured by the thermocompression treatment of the copper foil having a surface roughness of 0.706 μm as shown in FIG. 4, and the peel force of the same copper foil as measured by the thermocompression treatment of the untreated L CP film was 0.54N/mm, which was significantly improved.
Example 3
The L CP film surface processing method of the embodiment comprises the following steps:
removing oil from L CP film by ultrasonic treatment in ethanol for 60 min;
swelling the L CP film subjected to oil removal treatment in strong alkali alcohol ether solution at 90 ℃ for 3min, wherein the sodium hydroxide, ethylene glycol monomethyl ether, hexanediol and water in the solution are respectively 20g, 17.3g, 1.3g and 1L;
etching the swollen L CP film in a mixed solution of sodium hydroxide and potassium permanganate at 90 ℃ for 10min, wherein the sodium hydroxide, the potassium permanganate and the water in the mixed solution are respectively 20g, 30g and 1L;
reducing the L CP film subjected to etching treatment in a mixed solution of sulfuric acid and sodium oxalate at 10 ℃ for 10min, wherein the amount of sulfuric acid, sodium oxalate and water in the mixed solution is respectively 50ml, 17g and 1L;
the reduced L CP film was washed and dried in an oven at 100 deg.C for 120min to give a treated L CP film.
The microstructure of the L CP film surface obtained in the example was changed from the original film (fig. 5A) surface as shown in fig. 5B, and the surface roughness (fig. 5D) was increased from 0.172 μm to 0.829 μm of the original film (fig. 5C). The L CP film obtained in the example was hot-pressed with a copper foil having a surface roughness of 0.706 μm, and the peel force was 0.71N/mm as shown in fig. 6, and was greatly improved compared with the peel force of 0.54N/mm as measured after the untreated L CP film was hot-pressed with the same copper foil.
Compared with the prior art, the L CP film with a relatively smooth surface is processed and roughened by the processing method, and then is combined with the copper foil to obtain the copper-clad plate with good combination force, so that the problem of low peeling strength of the existing copper-clad plate is solved, the blank of the surface processing method of the L CP film is made up, the operation is simple, the threshold is low, the production conditions and the equipment and the raw materials are cheap and easy to obtain, and the method is easy to realize and popularize.
While the foregoing is directed to embodiments of the present invention, it will be understood by those skilled in the art that various changes may be made without departing from the spirit and scope of the invention.
Claims (10)
1. A surface treatment method of L CP film is characterized by comprising the following steps:
heating and swelling the L CP film in an alcohol ether solution containing strong base, wherein the content of the strong base in the alcohol ether solution containing the strong base is 1-20 g/L, the content of ethers is 1-18 g/L, and the content of alcohols is 0.1-1.5 g/L;
etching the swollen L CP film in a first mixed solution formed by strong base and strong oxidant, wherein the solvent in the first mixed solution is water, the content of the strong base is 1-20 g/L, and the content of the strong oxidant is 4-30 g/L;
reducing the L CP film subjected to etching treatment in a second mixed solution formed by strong acid and oxalate, wherein the content of the strong acid in the second mixed solution is 10-50 ml/L, and the content of the oxalate in the second mixed solution is 3-18 g/L;
the reduced L CP film was washed and dried.
2. The processing method according to claim 1, characterized in that: the strong base is at least one of potassium hydroxide, sodium hydroxide and lithium hydroxide.
3. The processing method according to claim 1, characterized in that: the solvent of the alcohol ether solution is at least one of ethylene glycol methyl ether, ethylene glycol ethyl ether, ethylene glycol, propylene glycol and hexylene glycol.
4. The processing method according to claim 1, characterized in that: the strong oxidant is at least one of potassium manganate, potassium permanganate and potassium dichromate.
5. The processing method according to claim 1, characterized in that: the strong acid is at least one of hydrochloric acid, nitric acid and concentrated sulfuric acid.
6. The processing method according to claim 1, characterized in that: the oxalate is at least one of ammonium oxalate, sodium oxalate and potassium oxalate.
7. The processing method according to claim 1, characterized in that: the temperature of the heating swelling treatment is 40-90 ℃, and the treatment time is 3-30 min.
8. The processing method according to claim 1, characterized in that: the etching treatment temperature is 40-90 ℃, and the treatment time is 10-120 min.
9. The processing method according to claim 1, characterized in that: the reduction treatment temperature is 10-50 ℃, and the treatment time is 1-10 min.
10. The processing method according to claim 1, characterized in that: the temperature of the drying treatment is 100-200 ℃, and the time is 30-120 min.
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2019
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| US20020155280A1 (en) * | 2000-07-18 | 2002-10-24 | 3M Innovative Properties Company | Liquid crystal polymers for flexible circuits |
| CN1550124A (en) * | 2001-09-04 | 2004-11-24 | 3M创新有限公司 | Liquid crystal polymers for flexible circuits |
| CN1709949A (en) * | 2004-06-18 | 2005-12-21 | Mec株式会社 | Resin surface treating agent and resin surface treatment |
| CN1994033A (en) * | 2004-07-29 | 2007-07-04 | 三井金属矿业株式会社 | Printed-circuit board, its manufacturing method and semiconductor device |
| CN102438405A (en) * | 2011-11-29 | 2012-05-02 | 电子科技大学 | Method for cleaning through hole smears of rigid-flexible printed circuit board |
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Application publication date: 20200807 |