CN108977770A - The surface treatment method of copper evaporation material - Google Patents
The surface treatment method of copper evaporation material Download PDFInfo
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- CN108977770A CN108977770A CN201710397730.3A CN201710397730A CN108977770A CN 108977770 A CN108977770 A CN 108977770A CN 201710397730 A CN201710397730 A CN 201710397730A CN 108977770 A CN108977770 A CN 108977770A
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- copper
- evaporation material
- pickling
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- treatment method
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F3/00—Brightening metals by chemical means
- C23F3/04—Heavy metals
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- 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
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/02—Cleaning or pickling metallic material with solutions or molten salts with acid solutions
- C23G1/10—Other heavy metals
- C23G1/103—Other heavy metals copper or alloys of copper
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- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
Abstract
The present invention provides a kind of surface treatment method of copper evaporation material, comprising: provides copper evaporation material；Material is evaporated to the copper and carries out the first pickling operation；After first pickling operation, centrifugation grinding operation is carried out to copper evaporation material；After the centrifugation grinding operation, material is evaporated to the copper and carries out cleaning operation；After the cleaning operation, copper evaporation material is dried.After the first pickling operation, centrifugation grinding operation is carried out to copper evaporation material, the centrifugation grinding operation can remove Cu oxide, the surface roughness for reducing the copper evaporation material, the surface brightness for improving the copper evaporation material and the smoothness, the surface micropore for reducing the copper evaporation material on the copper evaporation material surface, to reduce the contact area of copper the evaporation material and air, improve the oxidation resistance of the copper evaporation material, and then improve the purity of the copper evaporation material, the quality and performance for correspondingling increase the copper evaporation material, are improved coating quality.
Description
Technical field
The present invention relates to field of semiconductor manufacture more particularly to a kind of surface treatment methods of copper evaporation material.
Background technique
Physical vapour deposition (PVD) (Physical Vapor Deposition, PVD) be it is a kind of under vacuum conditions, use is low
The arc-discharge technique of voltage, high current evaporates target or evaporation material using gas discharge and makes to be evaporated substance and gas
It all ionizes, using the acceleration of electric field, makes to be evaporated substance and reactant is deposited on substrate.Currently, PVD technique
Have become semiconductor chip manufacturing industry, solar energy industry, LCD (Liquid Crystal Display, liquid crystal display) manufacture
The core technology of a variety of industries such as industry.
PVD technique mainly includes sputtering technology and evaporation coating techniques.Wherein, in vacuum environment, evaporation material is heated,
Evaporation, and be plated to the technology on substrate and be known as evaporation coating techniques.Currently, have a wide range of application since evaporation coating techniques have,
The advantages that pollution level is small is increasingly favored by technical staff in the industry.
The copper evaporation material of semiconductor integrated circuit is the indispensable raw material of wafer back technology for gold, still, the prior art
The quality and performance of copper evaporation material are poor, so as to cause the decline of coating quality.
Summary of the invention
Problems solved by the invention is to provide a kind of surface treatment method of copper evaporation material, improve copper evaporation material quality and
Performance.
To solve the above problems, the present invention provides a kind of surface treatment method of copper evaporation material, comprising: provide copper evaporation
Material；Material is evaporated to the copper and carries out the first pickling operation；After first pickling operation, copper evaporation material is centrifuged
Grinding operation；After the centrifugation grinding operation, material is evaporated to the copper and carries out cleaning operation；It is right after the cleaning operation
The copper evaporation material is dried.
Optionally, the step of first pickling operation includes: and evaporates material to the copper using the first pickling solution to carry out
First pickling；After evaporating material to the copper and carrying out the first pickling, material is evaporated to the copper using pure water and carries out the first ultrasonic wave
Cleaning.
Optionally, first pickling solution is dilute nitric acid solution.
Optionally, the volumetric concentration of the dilute nitric acid solution is 20% to 40%, and the pickling time of first pickling is 1
Minute was to 2 minutes.
Optionally, the scavenging period of first ultrasonic cleaning is 10 minutes to 15 minutes.
Optionally, to the copper evaporation material carry out centrifugation grinding operation the step of include: offer centrifugal grinder, it is described from
Heart grinder includes grinding drum；Copper evaporation material is placed in the grinding drum；Lapping liquid is added into the grinding drum；To
It is equipped in the grinding drum of the copper evaporation material and lapping liquid and water is added；After water is added, the grinding drum is packed into grinder, it is right
The copper evaporation material carries out centrifugation grinding.
Optionally, the ratio for the volume that the volume of the copper evaporation material accounts for the grinding drum is less than or equal to 2/3.
Optionally, the ratio for the volume that the volume of the copper evaporation material accounts for the grinding drum is 1/3 to 2/3.
Optionally, the lapping liquid is the detergent containing cocounut oil diglycollic amide.
Optionally, the lapping liquid is dish washing liquid or hand cleanser.
Optionally, the volume of the lapping liquid is 10 milliliters to 20 milliliters.
Optionally, in the step of centrifugation is ground, the revolving speed of the grinding drum is 150 revs/min to 170 revs/min
Clock, milling time are 10 minutes to 15 minutes.
Optionally, after water being added into the grinding drum for being equipped with the copper evaporation material and lapping liquid, the water surface to the grinding drum
The distance at top is 1 centimetre to 2 centimetres.
It optionally, further include step before evaporating material progress cleaning operation to the copper after the centrifugation grinding operation
It is rapid: material being evaporated to the copper and carries out the second pickling operation.
Optionally, the step of second pickling operation includes: and evaporates material to the copper using the second pickling solution to carry out
Second pickling；After evaporating material the second pickling of progress to the copper, it is clear that the second ultrasonic wave is carried out to copper evaporation material using pure water
It washes.
Optionally, second pickling solution is dilution heat of sulfuric acid or dilute hydrochloric acid solution.
Optionally, second pickling solution is dilution heat of sulfuric acid, the volumetric concentration of the dilution heat of sulfuric acid be 20% to
30%, the pickling time of second pickling is 1 minute to 2 minutes.
It optionally, further include step before evaporating material progress cleaning operation to the copper after second pickling operation
It is rapid: material being evaporated to the copper using pure water and carries out the second ultrasonic cleaning.
Optionally, the scavenging period of second ultrasonic cleaning is 10 minutes to 15 minutes.
Optionally, cleaning solution used by the cleaning operation is aqueous isopropanol or absolute alcohol.
Optionally, the scavenging period of the cleaning operation is 5 minutes to 15 minutes.
Optionally, withering step, which includes: to dry up the copper evaporation material using air gun, is expected to copper evaporation；
After drying up the copper evaporation material using air gun, copper evaporation material is dried in vacuo.
Optionally, in the vacuum drying the step of, vacuum degree is less than or equal to 10-2Pa。
Optionally, in the vacuum drying the step of, drying temperature is 60 DEG C to 80 DEG C, drying time be 1H extremely
1.5H。
Compared with prior art, technical solution of the present invention has the advantage that
After the first pickling operation, centrifugation grinding operation is carried out to copper evaporation material, the centrifugation grinding operation is in removal institute
State the residual pickling solution of the first pickling operation, removal residual it is water stain while, the copper on copper evaporation material surface can be removed
Oxide, the surface roughness for reducing the copper evaporation material, the surface brightness and smoothness, reduction for improving the copper evaporation material
The surface micropore of the copper evaporation material improves the copper evaporation material to reduce the contact area of copper the evaporation material and air
Oxidation resistance, and then improve the purity of copper evaporation material, the purity of the copper evaporation material made to can achieve 5N
(99.999%) or more, the quality and performance of the copper evaporation material are correspondinglyd increase, coating quality is improved.
In optinal plan, after the centrifugation grinding operation, before evaporating material progress cleaning operation to the copper, further include
Step: material is evaporated to the copper and carries out the second pickling operation；Second pickling operation can be used for further dissolving the oxidation of copper
Object and the residual impurity on copper evaporation material surface, to further improve the cleanliness of the copper evaporation material, and then advantageous
In the quality and performance that improve the copper evaporation material.
Detailed description of the invention
Fig. 1 is the flow diagram of one embodiment of surface treatment method of copper evaporation material of the present invention；
Fig. 2 is the perspective view of the evaporation of copper corresponding to step S1 material in embodiment illustrated in fig. 1；
Fig. 3 is structural schematic diagram corresponding to step S3 in embodiment illustrated in fig. 1.
Specific embodiment
It can be seen from background technology that the quality and performance of copper evaporation material are poor, so as to cause the decline of coating quality.Analyze copper
The reason that the quality and performance of evaporation material are poor is:
The surface treatment method of copper evaporation material mainly includes the pickling operation, cleaning operation and drying process successively carried out.
But copper is oxidizable material, therefore after pickling operation, and the copper evaporation material is easy to appear problem of oxidation, so as to cause the copper
The purity decline of evaporation material.
In evaporation coating techniques, in the use process of copper evaporation material, need to ensure copper evaporation material high-purity and
Cleanliness, therefore when problem of oxidation occurs in copper evaporation material, accordingly also result in the decline of coating quality.
In order to solve the technical problem, the present invention carries out centrifugation grinding behaviour after the first pickling operation, to copper evaporation material
Make, the centrifugation grinding operation can remove the Cu oxide on the copper evaporation material surface, reduce the surface of the copper evaporation material
Roughness, the surface brightness for improving the copper evaporation material and smoothness, the surface micropore for reducing the copper evaporation material, to drop
The contact area with air is expected in the low copper evaporation, and then improves the oxidation resistance of the copper evaporation material, and then described in raising
The purity of copper evaporation material.
To make the above purposes, features and advantages of the invention more obvious and understandable, with reference to the accompanying drawing to the present invention
Specific embodiment be described in detail.
With reference to Fig. 1, the flow diagram of one embodiment of surface treatment method of copper evaporation material of the present invention, this implementation are shown
Example surface treatment method includes following basic step:
Step S1: copper evaporation material is provided；
Step S2: material is evaporated to the copper and carries out the first pickling operation；
Step S3: after first pickling operation, centrifugation grinding operation is carried out to copper evaporation material；
Step S4: after the centrifugation grinding operation, material is evaporated to the copper and carries out cleaning operation；
Step S5: after the cleaning operation, copper evaporation material is dried.
Specific embodiments of the present invention are described further below in conjunction with attached drawing.
Step S1 is executed in conjunction with reference Fig. 2 with reference to Fig. 1, copper evaporation material 100 is provided.
The copper evaporation material 100 is for the raw material as evaporation coating techniques.
Depending on the shape of the copper evaporation material 100 can be required according to application environment and technique.In the present embodiment, the copper
The shape of evaporation material 100 is cuboid.
In a specific embodiment, the size of the copper evaporation material 100 is 10 millimeters × 10 millimeters × 2 millimeters.But
The present invention evaporates the size of material 100 without limitation to the copper.
In other embodiments, the shape of the copper evaporation material can also be square, cylindrical body or any other rule
Shape or irregular shape.For example, the copper evaporation material is the cylindrical body that diameter is 6 millimeters, length is 6 millimeters.
In the present embodiment, by taking the size of copper evaporation material 100 is 10 millimeters × 10 millimeters × 2 millimeters as an example, by copper ingot
By blanking, forge, roll, cut, the copper sheets of 2 millimeters thicks is made in the processes such as surface sand-blasting, then the copper sheet is fallen with punching press
10 millimeters × 10 millimeters × 2 millimeters of square piece is made in the mode of material, to expect 100 as copper evaporation.
Same as the prior art to the technique that the copper evaporation material 100 is made, the present embodiment no longer illustrates herein.
Wherein, the copper evaporation material 100 is obtained by blanking punched mode, therefore the number of copper evaporation material 100
It is multiple for measuring, and during subsequent technique, is surface-treated to multiple copper evaporation material 100.
It continues to refer to figure 1, executes step S2,100 the first pickling operations of progress (as shown in Figure 2) of material are evaporated to the copper.
First pickling operation is used to remove impurity and the dissolution copper evaporation on 100 surfaces of the copper evaporation material
Expect the Cu oxide on 100 surfaces.
Specifically, the step of first pickling operation include: using the first pickling solution to the copper evaporation material 100 into
The first pickling of row；After carrying out the first pickling to copper evaporation material 100, the is carried out to copper evaporation material 100 using pure water
One ultrasonic cleaning.
Wherein, the step of first pickling includes: and copper evaporation material 100 is put into pickling basket, then will be equipped with institute
The pickling basket for stating copper evaporation material 100 is put into the descaling bath for filling the first pickling solution, is made described in 100 immersion of copper evaporation material
In first pickling solution.
First pickling solution is the acid solution that can be reacted with copper product, to dissolve Cu oxide.This reality
It applies in example, first pickling solution is dilute nitric acid solution.
The volumetric concentration of the dilute nitric acid solution is unsuitable too small, also should not be too large.If the volume of the dilute nitric acid solution
Concentration is too small, then the effect of the impurity and Cu oxide that remove 100 surfaces of the copper evaporation material is poor；If the dust technology
The volumetric concentration of solution is excessive, accordingly will increase process dangerous.For this purpose, in the present embodiment, the volume of the dilute nitric acid solution
Concentration is 20% to 40%.
The pickling time of first pickling is unsuitable too short, also unsuitable too long.If the pickling time is too short, remove
The impurity on 100 surfaces of the copper evaporation material and the effect of Cu oxide are poor；If the pickling time is too long, cause instead
The waste of process time and cost, and reacted since the pickling solution can evaporate material 100 with the copper, it is also easy to lead
The problem for causing 100 losses of the copper evaporation material excessive.For this purpose, the pickling time of first pickling is 1 minute in the present embodiment
To 2 minutes.
After carrying out the first pickling to copper evaporation material 100 using the first pickling solution, 100 surfaces of copper evaporation material tool
There is first pickling solution, therefore after first pickling, the first ultrasound is carried out to copper evaporation material 100 using pure water
Wave cleaning, to remove first pickling solution of residual on 100 surfaces of the copper evaporation material.
Specifically, the pickling basket is put into pure water, after taking out in the descaling bath to described by the pickling basket
Copper evaporation material 100 carries out the first ultrasonic cleaning.
In the present embodiment, while guaranteeing cleaning effect, the waste of process time, first ultrasonic cleaning are avoided
Scavenging period be 10 minutes to 15 minutes.
It continues to refer to figure 1, and combines and refer to Fig. 3, Fig. 3 is structural representation corresponding to step S3 in embodiment illustrated in fig. 1
Figure executes step S3, after first pickling operation, carries out centrifugation grinding operation to copper evaporation material 100.
The centrifugation grinding operation is used to play the role of surface polishing to copper evaporation material 100, thus described in removal
The Cu oxide on 100 surfaces of copper evaporation material, improves the copper evaporation material 100 at the surface roughness for reducing the copper evaporation material 100
Surface brightness and smoothness, the surface micropore for reducing copper evaporation material 100, with reduce the copper evaporation material 100 with it is empty
The contact area of gas, and then improve the oxidation resistance of the copper evaporation material 100.
In addition, by the centrifugation grinding operation, the residual the on 100 surfaces of the copper evaporation material can also be further removed
Residual after one pickling solution, first ultrasonic cleaning is water stain and dirty.
Specifically, the step of carrying out centrifugation grinding operation to copper evaporation material 100 includes: to provide centrifugal grinder (figure
Do not show), the centrifugal grinder includes grinding drum 200；Copper evaporation material 100 is placed in the grinding drum 200；To described
Lapping liquid (not shown) is added in grinding drum 200；It is added into the grinding drum 200 for being equipped with the copper evaporation material 100 and lapping liquid
Water 300；After water 300 is added, the grinding drum 200 is packed into grinder, centrifugation grinding is carried out to copper evaporation material 100.
The centrifugation grinding operation utilizes the principle of centrifugal movement, between water and copper evaporation material 100 and described
The lower generation grinding motion of mutual extrusion effect between copper evaporation material 100, and grinding rate with higher, evaporate the copper
Material 100 has the function that high speed grinding polishes under centrifugation rotation, to remove the burr and copper on 100 surfaces of the copper evaporation material
Oxide, and play the role of polishing, and then improve the surface smoothness of the copper evaporation material 100.
The centrifugal grinder is same as the prior art, and to the specific descriptions of the centrifugal grinder, the present embodiment is herein
It repeats no more.
It should be noted that being usually also equipped with ceramic grinding material, the material of the ceramic grinding material in the grinding drum 200
Aluminium impurity, therefore the present embodiment are readily incorporated when carrying out the centrifugation grinding operation using the ceramic grinding material for aluminium oxide
In, in the case where not using the ceramic grinding material, carry out the centrifugation grinding operation.
In the present embodiment, after copper evaporation material 100 is placed in the grinding drum 200, the body of the copper evaporation material 100
The ratio that product accounts for the volume of the grinding drum 200 is less than or equal to 2/3.If the volume of the copper evaporation material 100 accounts for described grind
The ratio of the volume of grinding barrel 200 is greater than 2/3, and the ratio that accordingly will cause water is too small, to be easy to cause the centrifugation grinding behaviour
It is difficult to be normally carried out, and then causes the effect for reducing the surface roughness of the copper evaporation material 100 poor.
If the ratio for the volume that the volume of the copper evaporation material 100 accounts for the grinding drum 200 is smaller, the grinding drum
200 utilization rate is lower, correspondingly, grinding efficiency is also lower.For this purpose, guaranteeing the centrifugation grinding operation in the present embodiment
Technological effect while, improve the utilization rate of the grinding drum 200 as far as possible, the volume of the copper evaporation material 100 accounts for described grind
The ratio of the volume of grinding barrel 200 is 1/3 to 2/3.
The effect of the lapping liquid includes: the Cu oxide on 100 surfaces of the dispersion copper evaporation material, to make the copper oxygen
Compound is easy to evaporate material 100 surface grindings removal from the copper, to improve grinding efficiency；It is risen between copper evaporation material 100
To lubricating action, to make the copper evaporation material 100 obtain bright and clean surface after the centrifugation grinding operation；Inhibition falls off
Rear Cu oxide, dirty etc. are re-attached to 100 surfaces of the copper evaporation material；The lapping liquid is also used to remove the copper and steams
First pickling solution of residual on 100 surface of material issuance；In addition, during the centrifugation grinding operation, the lapping liquid and water
It stirs together, is conducive to alleviate the mutual shock between the copper evaporation material 100.
The lapping liquid is the organic solution with dirt-removing power, so as to remove 100 surfaces of the copper evaporation material
Cu oxide, while improve the surface brightness and smoothness of copper evaporation material 100, preferably remove the copper evaporation
Expect that the first pickling solution of residual, the residual on 100 surfaces are water stain and dirty.
In the present embodiment, the lapping liquid is the detergent containing cocounut oil diglycollic amide, the cocounut oil diglycollic amide
Dirt-removing power for nonionic surfactant, the cocounut oil diglycollic amide is stronger, therefore the lapping liquid suppression can be improved
Make the dirty ability for being re-attached to 100 surfaces of the copper evaporation material.
In the present embodiment, the lapping liquid is hand cleanser.Such as hands washing solution for workers can be used.In other embodiments,
The lapping liquid can also be dish washing liquid.
The volume of the lapping liquid is unsuitable too small, also should not be too large.If the volume of the lapping liquid is too small, it is easy to lead
Cause the ineffective of removal pickling solution；If the volume of the lapping liquid is excessive, reaching preferably removal pickling solution
In the case where effect, the waste of the lapping liquid is caused.For this purpose, in the present embodiment, the volume of the lapping liquid be 10 milliliters extremely
20 milliliters.
Water has the function of buffering in the centrifugation grinding operation and clean that the additive amount of water is more, and buffer function is big, institute
The degree of deformation for stating copper evaporation material 100 is smaller, and advantageously reduces the surface roughness of the copper evaporation material 100.In the present embodiment,
After water 300 is added into the grinding drum 200 for being equipped with the copper evaporation material 100 and lapping liquid, the water surface to 200 top of grinding drum
Distance (not indicating) be 1 centimetre to 2 centimetres.It in other embodiments, can also be by the built-in full water of the grinding drum, the i.e. water surface
It is flushed at the top of the grinding drum.
The centrifugation grinding operation has the function that polishing, therefore the grinding drum 200 using the principle of centrifugal movement
Revolving speed it is bigger, the effect for reducing copper evaporation 100 surface roughnesses of material is better；But the revolving speed of the grinding drum 200 is not
Preferably excessive, the hardness of copper product is lower, if the revolving speed of the grinding drum 200 is excessive, the corner angle of the copper evaporation material 100 are easy
Crimping is generated because of shock, and impurity is easy to accumulate in the crimping area defined, steam to reduce the copper
The quality of material issuance 100.For this purpose, in the step of centrifugation is ground, the revolving speed of the grinding drum 200 is 150 in the present embodiment
Rev/min to 170 revs/min.
Correspondingly, the milling time of the centrifugation grinding is longer, the effect of copper evaporation 100 surface roughnesses of material is reduced
Better；But if time consuming is too long, in the case where reaching preferable grinding effect, the process time is wasted instead, is caused into
This waste.For this purpose, in the step of centrifugation is ground, milling time is 10 minutes to 15 minutes in the present embodiment.
It should be noted that further comprising the steps of: after the centrifugation grinding operation and evaporating 100 (such as Fig. 3 of material to the copper
It is shown) carry out the second pickling operation.
Aforementioned first pickling operation is used to remove the Cu oxide and impurity on 100 surfaces of the copper evaporation material, in order to anti-
Only 100 surfaces of copper evaporation material have remaining Cu oxide and impurity, therefore by second pickling operation, with into
One step removes the Cu oxide and impurity.
Specifically, the step of second pickling operation include: using the second pickling solution to the copper evaporation material 100 into
The second pickling of row；After carrying out the second pickling to copper evaporation material 100, second is carried out to copper evaporation material 100 using pure water
Ultrasonic cleaning.
Wherein, the step of second pickling includes: and copper evaporation material 100 is put into pickling basket, then will be equipped with institute
The pickling basket for stating copper evaporation material 100 is put into the descaling bath for filling the second pickling solution, is made described in 100 immersion of copper evaporation material
In second pickling solution.
In order to reduce consumption of second pickling to copper evaporation material 100, second pickling solution and copper product
Respond it is smaller, or do not react with copper product, but second pickling solution can dissolve Cu oxide and impurity.
Therefore second pickling solution can be dilution heat of sulfuric acid or dilute hydrochloric acid solution, and second pickling solution may be used also
Think other acid solutions not reacted with copper product.
In the present embodiment, second pickling solution is dilution heat of sulfuric acid.
The volumetric concentration of the dilution heat of sulfuric acid is unsuitable too small, also should not be too large.If the volume of the dilution heat of sulfuric acid
Concentration is too small, then the effect of the residual impurity and Cu oxide that remove 100 surfaces of the copper evaporation material is poor；If described dilute
The volumetric concentration of sulfuric acid solution is excessive, and the pickling solution is easy to react with copper evaporation material 100, causes calmly described
The loss of copper evaporation material 100, and volumetric concentration is excessive accordingly also will increase process dangerous.For this purpose, in the present embodiment, it is described dilute
The volumetric concentration of sulfuric acid solution is 20% to 30%.
The pickling time of second pickling is unsuitable too short, also unsuitable too long.If the pickling time is too short, remove
The residual impurity on 100 surfaces of the copper evaporation material and the effect of Cu oxide are poor；If the pickling time is too long, instead
Cause the waste of process time and cost.For this purpose, the pickling time of second pickling is 1 minute to 2 points in the present embodiment
Clock.
After carrying out the second pickling to copper evaporation material 100 using second pickling solution, copper evaporation 100 tables of material
Face has second pickling solution, therefore after second pickling, carries out second to copper evaporation material 100 using pure water
Ultrasonic cleaning, to remove second pickling solution of residual on 100 surfaces of the copper evaporation material.
Specifically, the pickling basket is put into pure water, after taking out in the descaling bath to described by the pickling basket
Copper evaporation material 100 carries out the second ultrasonic cleaning.
In the present embodiment, while guaranteeing cleaning effect, the waste of process time, second ultrasonic cleaning are avoided
Scavenging period be 10 minutes to 15 minutes.
It continues to refer to figure 1, executes step S4, after the centrifugation grinding operation, to copper evaporation material 100 (such as Fig. 2 institute
Show) carry out cleaning operation.
Achieve the effect that dehydration by the cleaning operation to remove the moisture on 100 surfaces of the copper evaporation material,
To provide Process ba- sis for subsequent drying process.
For this purpose, cleaning solution used by the cleaning operation is for isopropanol (IPA) solution or without watery wine in the present embodiment
Essence.
It should be noted that the scavenging period of the cleaning operation is unsuitable too short, it is also unsuitable too long.If when the cleaning
Between it is too short, then the effect of dehydration is poor；If the scavenging period is too long, in the feelings for reaching preferable dehydration effect
Under condition, the process time is wasted instead.For this purpose, the scavenging period of the cleaning operation is 5 minutes to 15 minutes in the present embodiment.
It continues to refer to figure 1, executes step S5, after the cleaning operation, 100 (as shown in Figure 2) of material are evaporated to the copper
It is dried.
By the way that copper evaporation material 100 is dried, evaporate what material 100 aoxidized again to improve the copper
Problem.
Specifically, evaporating 100 withering steps of material to the copper includes: to dry up the copper evaporation using air gun
Material 100；After drying up the copper evaporation material 100 using air gun, copper evaporation material 100 is dried in vacuo.
In the present embodiment, in the case where the visually copper evaporation 100 surface no moisture of material, stop using the air gun
Movement improves vacuum drying efficiency to provide Process ba- sis for subsequent vacuum drying.
In the present embodiment, the vacuum drying the step of in, vacuum degree is less than or equal to 10-2Pa.When the vacuum degree
Greater than 10-2When Pa, it is easy to increase a possibility that copper evaporation material 100 aoxidizes.
It should be noted that drying temperature is unsuitable too low in the vacuum drying the step of, it otherwise be easy to cause vacuum
The decline of drying efficiency；But when the drying temperature is excessively high, it is easy to increase process risk, is also easy to vacuum dryer
Stability generate adverse effect.For this purpose, the vacuum drying drying temperature is 60 DEG C to 80 DEG C in the present embodiment.
It should also be noted that, drying time is unsuitable too short in the vacuum drying the step of, it is also unsuitable too long.Such as
Drying time described in fruit is too short, in the case where drying temperature is certain, is easy to cause drying process insufficient, so as to cause described
Copper evaporation material 100 is easy to happen oxidation；If the drying time is too long, in the case where reaching preferable drying effect, instead
Waste process time and the energy.For this purpose, the vacuum drying drying time is 1H (hour) to 1.5H in the present embodiment.
In addition, the copper evaporation material 100 aoxidizes again in order to prevent, after the drying process, the copper is prevented
Evaporation material 100 is chronically exposed in wet environment.Wherein, as long as guaranteeing the copper evaporation material 100 in normal room humidity ring
Under border.Such as: in the present embodiment, makes the copper evaporation material 100 in clean room environment, control the wet of the dust free room
Degree is 30% to 50%.
Although of the invention, oneself is disclosed as above, and present invention is not limited to this.Anyone skilled in the art are not departing from
It in the spirit and scope of the present invention, can make various changes or modifications, therefore protection scope of the present invention should be with claim
Subject to limited range.
Claims (23)
1. a kind of surface treatment method of copper evaporation material characterized by comprising
Copper evaporation material is provided；
Material is evaporated to the copper and carries out the first pickling operation；
After first pickling operation, centrifugation grinding operation is carried out to copper evaporation material；
After the centrifugation grinding operation, material is evaporated to the copper and carries out cleaning operation；
After the cleaning operation, copper evaporation material is dried.
2. surface treatment method as described in claim 1, which is characterized in that the step of first pickling operation includes: to adopt
The first pickling is carried out to copper evaporation material with the first pickling solution；
After evaporating material to the copper and carrying out the first pickling, material is evaporated to the copper using pure water and carries out the first ultrasonic cleaning.
3. surface treatment method as claimed in claim 2, which is characterized in that first pickling solution is dilute nitric acid solution.
4. surface treatment method as claimed in claim 3, which is characterized in that the volumetric concentration of the dilute nitric acid solution is 20%
To 40%, the pickling time of first pickling is 1 minute to 2 minutes.
5. surface treatment method as claimed in claim 2, which is characterized in that the scavenging period of first ultrasonic cleaning is
10 minutes to 15 minutes.
6. surface treatment method as described in claim 1, which is characterized in that carry out centrifugation grinding operation to copper evaporation material
The step of include: offer centrifugal grinder, the centrifugal grinder includes grinding drum；
Copper evaporation material is placed in the grinding drum；
Lapping liquid is added into the grinding drum；
Water is added into the grinding drum for being equipped with the copper evaporation material and lapping liquid；
After water is added, the grinding drum is packed into grinder, centrifugation grinding is carried out to copper evaporation material.
7. surface treatment method as claimed in claim 6, which is characterized in that the volume of the copper evaporation material accounts for the grinding drum
Volume ratio be less than or equal to 2/3.
8. surface treatment method as claimed in claims 6 or 7, which is characterized in that the volume of the copper evaporation material accounts for described grind
The ratio of the volume of grinding barrel is 1/3 to 2/3.
9. surface treatment method as claimed in claim 6, which is characterized in that the lapping liquid is to contain cocounut oil diglycollic amide
Detergent.
10. the surface treatment method as described in claim 6 or 9, which is characterized in that the lapping liquid is dish washing liquid or washes one's hands
Liquid.
11. surface treatment method as claimed in claim 6, which is characterized in that the volume of the lapping liquid is 10 milliliters to 20
Milliliter.
12. surface treatment method as claimed in claim 6, which is characterized in that described to grind in the step of centrifugation is ground
The revolving speed of grinding barrel is 150 revs/min to 170 revs/min, and milling time is 10 minutes to 15 minutes.
13. surface treatment method as claimed in claim 6, which is characterized in that expect and lapping liquid to the copper evaporation is equipped with
After water is added in grinding drum, the distance at the top of the water surface to the grinding drum is 1 centimetre to 2 centimetres.
14. surface treatment method as described in claim 1, which is characterized in that after the centrifugation grinding operation, to the copper
Before evaporation material carries out cleaning operation, further comprises the steps of: to evaporate the copper and expect to carry out the second pickling operation.
15. surface treatment method as claimed in claim 14, which is characterized in that the step of second pickling operation includes:
Material is evaporated to the copper using the second pickling solution and carries out the second pickling；
After evaporating material the second pickling of progress to the copper, material is evaporated to the copper using pure water and carries out the second ultrasonic cleaning.
16. surface treatment method as claimed in claim 15, which is characterized in that second pickling solution is dilution heat of sulfuric acid
Or dilute hydrochloric acid solution.
17. surface treatment method as claimed in claim 15, which is characterized in that second pickling solution is that dilute sulfuric acid is molten
Liquid, the volumetric concentration of the dilution heat of sulfuric acid are 20% to 30%, and the pickling time of second pickling is 1 minute to 2 minutes.
18. surface treatment method as claimed in claim 15, which is characterized in that the scavenging period of second ultrasonic cleaning
It is 10 minutes to 15 minutes.
19. surface treatment method as described in claim 1, which is characterized in that cleaning solution used by the cleaning operation
For aqueous isopropanol or absolute alcohol.
20. surface treatment method as claimed in claim 19, which is characterized in that the scavenging period of the cleaning operation is 5 points
Clock was to 15 minutes.
21. surface treatment method as described in claim 1, which is characterized in that withering to copper evaporation material
Step includes: to dry up the copper evaporation material using air gun；
After drying up the copper evaporation material using air gun, copper evaporation material is dried in vacuo.
22. surface treatment method as claimed in claim 21, which is characterized in that in the vacuum drying the step of, vacuum
Degree is less than or equal to 10-2Pa。
23. the surface treatment method as described in claim 21 or 22, which is characterized in that in the vacuum drying the step of,
Drying temperature is 60 DEG C to 80 DEG C, and drying time is 1H to 1.5H.
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| CN111394697A (en) * | 2020-04-27 | 2020-07-10 | 宁波江丰电子材料股份有限公司 | Surface treatment method of metal evaporation material |
| CN111876787A (en) * | 2020-07-22 | 2020-11-03 | 宁波江丰电子材料股份有限公司 | Treatment process of copper phosphorus evaporation material |
| CN112223099A (en) * | 2020-10-12 | 2021-01-15 | 宁波江丰电子材料股份有限公司 | Surface cleaning method for sulfur-containing nickel beads of electroplating anode material |
| CN113290427A (en) * | 2021-05-24 | 2021-08-24 | 宁波江丰电子材料股份有限公司 | Treatment method of high-purity nickel evaporation material |
| CN113480974A (en) * | 2021-08-04 | 2021-10-08 | 宁波江丰电子材料股份有限公司 | Grinding composition and application thereof |
| CN113664472A (en) * | 2021-08-25 | 2021-11-19 | 宁波江丰电子材料股份有限公司 | Preparation method of nickel evaporation material |
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Application publication date: 20181211 |