CN104947110A - Micro etchant, production method of circuit board and circuit board - Google Patents
Micro etchant, production method of circuit board and circuit board Download PDFInfo
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- CN104947110A CN104947110A CN201410119458.9A CN201410119458A CN104947110A CN 104947110 A CN104947110 A CN 104947110A CN 201410119458 A CN201410119458 A CN 201410119458A CN 104947110 A CN104947110 A CN 104947110A
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Abstract
The invention discloses a micro etchant, and a production method of a circuit board. The micro etchant comprises a first micro etchant component and a second micro etchant component, wherein the first micro etchant component contains sulphuric acid and hydrogen peroxide aqueous solution, the second micro etchant component is ammonia water, and the pH value of the mixed system of the first micro etchant component and the second etchant component is 2-4. Micro etching is carried out on a copper circuit layer of a ceramic substrate in one step only, so that production cost of the circuit board is reduced; adhesive strength between the copper circuit layer and a nickel layer on the ceramic substrate is high; besides, the circuit board disclosed by the invention has high heat conductivity and can be applied to a high power LED, an automotive headlamp and a high power assembly.
Description
Technical field
The present invention relates to the manufacture method of a kind of micro-etching agent and wiring board.
Background technology
On current LED market, the line layer of ceramic substrate is all layers of copper, by plating or typography in ceramic base plate surface copper circuits.Because the resistivity of silver is much lower compared with copper, so the useful copper slurry containing silver carries out printed wiring now, and existing ceramic substrate electroless plating pre-treating process only slightly stings erosion to copper, and do not relate to silver sting erosion, but the existence of silver suboxide makes the bonding force of copper wire layer and nickel dam after electroless plating completes very poor, all ruptures between copper wire layer and nickel dam during PULL Elongation test.Successively erosion all stung to the copper in copper wire layer and silver although CN102858093A discloses thus obtain the method for higher copper nickel bonding force, but the method needs to carry out microetch in two steps, both add cell body like this, extend the operating time again, cost is remained high.
Therefore, the manufacture method that a kind of new micro-etching agent and wiring board are provided is needed badly.
Summary of the invention
The object of the invention is to solve the problem containing bonding force difference between silver-colored copper wire layer and ceramic substrate in prior art, the manufacture method of a kind of micro-etching agent and wiring board is provided.
According to a first aspect of the invention, the invention provides a kind of micro-etching agent, described micro-etching agent comprises the first micro-etching agent component and the second micro-etching agent component, described first micro-etching agent component contains the aqueous solution of sulfuric acid and hydrogen peroxide, described second micro-etching agent component is ammoniacal liquor, and the pH value of the mixed system of described first micro-etching agent component and described second micro-etching agent component is 2-4.
According to a second aspect of the invention, the invention provides a kind of manufacture method of wiring board, described method comprises carries out microetch by the copper wire layer of micro-etching agent at least one surface being attached to ceramic substrate, and the surface of copper wire layer after microetch is formed nickel dam and optional palladium layers and layer gold, containing silver in described copper wire layer, wherein, described micro-etching agent is above-mentioned micro-etching agent.
The present invention carries out microetch to copper wire layer on ceramic substrate only needs a step to carry out, and therefore, reduces the manufacturing cost of wiring board.Ceramic substrate of the present invention has higher bonding force between copper wire layer and nickel dam.In addition, wiring board of the present invention also has higher thermal conductivity, can be applied in high-capacity LED, headlight for vehicles and high power component.
Other features and advantages of the present invention are described in detail in embodiment part subsequently.
Embodiment
According to a first aspect of the invention, the invention provides a kind of micro-etching agent, described micro-etching agent comprises the first micro-etching agent component and the second micro-etching agent component, described first micro-etching agent component contains the aqueous solution of sulfuric acid and hydrogen peroxide, described second micro-etching agent component is ammoniacal liquor, and the pH value of the mixed system of described first micro-etching agent component and described second micro-etching agent component is 2-4.
Described micro-etching agent can remove in the copper wire layer containing silver due to the cupric oxide of burning generation and silver suboxide.
In described micro-etching agent, the content of each component can be selected according to the degree of oxidation of copper wire layer.Usually, in described first micro-etching agent component, the concentration of sulfuric acid can be 40-120g/L, and the concentration of hydrogen peroxide can be 30-75g/L; In described second micro-etching agent component, the concentration of ammoniacal liquor can be 20-65g/L.Under preferable case, the concentration of sulfuric acid is 60-110g/L, and the concentration of hydrogen peroxide is 45-70g/L, and the concentration of ammoniacal liquor is 30-50g/L, can improve the etch-rate of described micro-etching agent so further, can reduce the consumption of micro-etching agent simultaneously.
In the present invention, in order to meet the processing requirement of microetch, the pH value of the mixed system of described first micro-etching agent component and described second micro-etching agent component is 2-4.
Described micro-etching agent can be obtained by the method for this area routine, such as, superoxol directly can be poured in sulphuric acid soln and obtain the first micro-etching agent, then when being about to carry out microetch to copper wire layer, add the second micro-etching agent containing ammonia soln again, obtain mixed system, finally the pH of mixed system can be regulated to be 2-3 with acetic acid or sodium carbonate, thus obtained fresh micro-etching agent.
Described sulphuric acid soln can be the sulphuric acid soln of any concentration.Be preferably the vitriol oil of concentration more than 70 % by weight, more preferably concentration is the vitriol oil of 98 % by weight.
Described hydrogen peroxide can be the superoxol of various concentration.Usually, in described superoxol, the concentration of hydrogen peroxide can be 5-35 % by weight.In the present invention, from the angle that raw material is easy to get, described hydrogen peroxide is preferably the superoxol that concentration is 30 % by weight.
Described ammoniacal liquor can be the ammonia soln of 20-30 % by weight for concentration, and in the present invention, preferred concentration is the ammoniacal liquor of 25 % by weight.
According to a second aspect of the invention, the invention provides a kind of manufacture method of wiring board, described method comprises carries out microetch by the copper wire layer of micro-etching agent at least one surface being attached to ceramic substrate, and the surface of copper wire layer after microetch is formed nickel dam and optional palladium layers and layer gold, containing silver in described copper wire layer, wherein, described micro-etching agent is above-mentioned micro-etching agent.
According to the present invention, described ceramic substrate can be the ceramic substrate of this area routine, such as, can be aluminum nitride ceramic substrate, aluminium oxide ceramic substrate or silicon carbide ceramics substrate.From the angle improving described wiring board heat-sinking capability, described ceramic substrate is preferably aluminum nitride ceramic substrate.
Copper wire layer on ceramic substrate of the present invention can obtain according to the method for this area routine.Usually, can thick film technology be adopted, namely utilize print process that copper slurry is coated substrate surface, then sinter through thermal treatment, copper slurry and obtain copper wire layer; Or use thin film technique, namely shaping by vacuum maskings such as sputtering, vacuum evaporations, ceramic base plate surface is metallized, forms described copper wire layer through photoetching, etching work procedure.Containing silver in described copper wire layer, the content of described silver is the selection of this area routine.Such as, in the copper for the formation of described copper wire layer is starched, the mass ratio that argent and copper are starched can be 1:3-6.In the present invention in following examples and comparative example, formed in the copper slurry of copper wire layer, the mass ratio that argent and copper are starched is 1:4.The concrete grammar forming described copper wire layer is the method for this area routine, does not repeat them here.
In the present invention, the process of described microetch can comprise: after the first microetch component in described micro-etching agent and the mixing of the second microetch component, described copper wire layer contacted to carry out microetch with the mixed system of described first microetch component with described second microetch component immediately.
In the present invention, the temperature of described microetch can be 15-35 DEG C; The time of described microetch can be 30-50s.
Well known to a person skilled in the art and be, before the copper wire layer being attached at least one surface of ceramic substrate is carried out microetch, need to use acid degreasing agent to carry out degreasing to described copper wire layer, the concrete grammar of described degreasing is the method for this area routine, does not repeat them here.
According to the present invention, the process forming nickel dam can comprise: carry out chemical nickel plating by chemical nickel-plating liquid to the surface of copper wire layer.Usually, ceramic substrate can be placed in the chemical nickel-plating liquid that temperature is 80-90 DEG C (as 83-86 DEG C), thus form nickel dam on the surface of the copper wire layer of substrate.The time of chemical nickel plating can be selected according to the thickness of the nickel dam of expection, can be generally 20-40min.
Nickel salt and reductive agent can be contained in described chemical nickel-plating liquid.The content of described reductive agent and described nickel salt can be the conventional content of this area.Such as, the content of described nickel salt can be 12-50g/L, and the content of described reductive agent can be 15-50g/L.Under preferable case, the content of described nickel salt is 20-40g/L, and the content of described reductive agent is 20-45g/L, and described chemical nickel-plating liquid can be made like this to have higher stability, and improves the bonding force between copper wire layer and nickel dam further.
The kind of the present invention to described nickel salt and reductive agent has no particular limits, and can be conventional selection.
Particularly, described nickel salt can be one or more in single nickel salt, nickelous chloride and nickel acetate, is preferably single nickel salt.
Described reductive agent can be sodium hypophosphite, potassium hypophosphite, POTASSIUM BOROHYDRIDE, sodium borohydride, hydrazine or dimethylamine borane.From the angle reducing described chemical nickel-plating liquid cost, described reductive agent is preferably sodium hypophosphite.
According to the present invention, described chemical nickel-plating liquid can also contain stablizer, complexing agent and buffer reagent, to avoid decomposition and the precipitation of chemical nickel-plating liquid.The present invention is not particularly limited the kind of described stablizer, complexing agent and buffer reagent and content thereof.
Described stablizer can be at least one in Sulfothiorine, Potassium Thiosulphate, thiocarbamide and xanthate, is preferably thiocarbamide.The content of described stablizer can be 0.5-5mg/L.
Described complexing agent can be at least one in succinic acid, Soduxin, citric acid, Trisodium Citrate, lactic acid, oxysuccinic acid, glycine, is preferably Trisodium Citrate.The content of described complexing agent can be 25-45g/L.
Described buffer reagent can be at least one in sodium-acetate, Soduxin and natrium hydrocitricum, is preferably sodium-acetate.The content of described buffer reagent can be 5-20g/L.
According to the present invention, in order to meet the requirement of chemical plating technology, the pH of described chemical nickel-plating liquid can be 3-5.
Be placed in by ceramic substrate before chemical nickel-plating liquid carries out chemical nickel plating, the surface of method to described copper wire layer that this area can be adopted to commonly use activates.The present invention is not particularly limited for the method for being carried out activating in the surface of described copper wire layer, and the ordinary method of this area can be adopted to carry out.
Usually, ceramic substrate can be put into containing palladium activator and aqueous acid, so that will the copper wire layer activation forming coating be needed.Described palladium activator can be palladous sulfate, and described acid is preferably sulfuric acid, and more preferably concentration is the sulfuric acid of 98 % by weight.The content of described palladium activator and acid can be conventional selection.Usually, the content of described palladium activator can be 0.2-2.5g/L, and concentration is the content of the sulfuric acid of 98 % by weight can be 55-90mL/L.PH value containing palladium activator and aqueous acid can be generally 3-5.
When activating, the temperature containing palladium activator and aqueous acid can be 25-35 DEG C.The time of described palladium activation can be generally 30-90 second.
According to the present invention, after the surface of described copper wire layer forms nickel dam, the nickel dam surface that described method can also be included in formation successively forms palladium layers and layer gold, and the method forming palladium layers and layer gold is the method for this area routine.
Particularly, the substrate that chemical nickel plating obtains can be placed in chemical palladium plating solution and carry out chemical palladium-plating, to form palladium layers on the surface of described nickel dam.Described chemical palladium plating solution can contain palladium salt, reductive agent, complexing agent and stablizer.Described palladium salt can be one or more in Palladous chloride, palladium bromide and palladous sulfate, described reductive agent can be sodium hypophosphite, hydrazine or dimethylamine borane, described complexing agent can be ethylenediamine tetraacetic acid (EDTA) and/or quadrol, and described stablizer can be one or more in ammonium chloride, Sulfothiorine and THIOGLYCOL acid.
In described chemical palladium plating solution, the content of described palladium salt can be 3-10g/L, and the content of described reductive agent can be 0.5-15g/L, and the content of described complexing agent can be 15-35g/L, and the content of described stablizer can be 5-20mg/L.
The condition of described chemical palladium-plating can comprise: pH value is 7-8, and temperature is 40-60 DEG C (as 45-55 DEG C).The treatment time of described chemical palladium-plating can be 7-20min, is preferably 8-10min.
The substrate that chemical palladium-plating obtains can be placed in chemical gold plating liquid, to form layer gold further on palladium layers surface.Described chemical gold plating liquid can contain golden salt, reductive agent and complexing agent.Described golden salt can be one or more in potassium auric cyanide, potassium cyanaurite and hydrochloro-auric acid, described reductive agent can be sodium hypophosphite, POTASSIUM BOROHYDRIDE, hydrazine or dimethylamine borane, and described complexing agent can be one or more in potassium cyanide, ethylenediamine tetraacetic acid (EDTA), thanomin and Sulfothiorine.
In described chemical gold plating liquid, the content of described golden salt can be 2-7g/L, and the content of described reductive agent can be 4-12g/L, and the content of described complexing agent can be 3-8g/L.
The condition of described chemical gilding can comprise: pH value is 7-8, and temperature is 80-85 DEG C.The treatment time of described chemical gilding can be 8-11min.
After carrying out each step electroless plating, ordinary method can be adopted to wash the substrate through electroless plating.Particularly, the tertiary effluent washing trough substrate after each step process can being put into lasting overflow processes 50-70s.
After electroless plating completes, can also comprise and the wiring board of preparation is carried out drying.The condition of described drying can be conventional selection.Such as, can first be dried up by the moisture of PCB surface, the baking oven then putting into 80-100 DEG C is dried.
In more detail the present invention will be described by embodiment below.
In following examples and comparative example, acid degreasing agent is purchased from Shenzhen Success Technology Co., Ltd., and the trade mark is CG-1551; The composition of chemical palladium plating solution and chemical gold plating liquid and content thereof are as shown in Table 1.
The thermal conductivity test of wiring board: adopt laser Conduction Coefficient Detector Basing (originating from German Nai Chi company, LFA447 type), probe temperature is 25 DEG C.
Stretch (PULL) strength test: wiring board sample is cut into foursquare each 5 pieces of 3mm in length and breadth, amount to 25 fritters, then on gold plate, a nailhead-shaped lead is welded, (to be paused Mechanical Equipment Company purchased from Shanghai Songyuan by tension testing machine after leaving standstill, model WDW-2) tensile strength test is carried out to sample and records tensile strength values, pulling rate is 10mm/min, peels off position and is designated as defective between layers of copper and nickel dam, record underproof number.
Table 1
Embodiment 1-3
Embodiment 1-3 is for illustration of wiring board provided by the invention and preparation method thereof.
Step 1 a: acid degreasing agent surface attachment being had the aluminum nitride ceramic substrate (76mm × 12.5mm × 0.5mm) of copper wire layer (thickness is 50 μm) to put into 100mL/L carries out degreasing, with the Temperature Treatment 6min of 45 DEG C.
Step 2: be placed with successively by the substrate after degreasing in the tertiary effluent washing trough of lasting overflow and process 50s, with processing procedure liquid medicine before thorough cleaning base plate remained on surface.
Step 3: substrate is put into immediately the first micro-etching agent (specifically forming in table 2) and mix formed fresh micro-etching agent with the second micro-etching agent (specifically forming in table 2), the pH controlling micro-etching agent is 2-3, with room temperature treatment 35s, to obtain fresh copper circuit surface.
Step 4: the substrate after microetch is placed with successively in the tertiary effluent washing trough of lasting overflow and processes 60s, processing procedure liquid medicine before residual with thorough clean plate face.
Step 5: the sulphuric acid soln (concentration is 98 % by weight) substrate being put into 35mL/L carries out acidification, and the treatment time is 50s, the substrate surface after activation microetch.
Step 6: the substrate after activation microetch is placed with in the tertiary effluent washing trough of lasting overflow successively and processes 60s, processing procedure liquid medicine before residual with thorough clean plate face.
Step 7: mixing solutions substrate being put into the sulfuric acid (concentration is 98 % by weight) of palladous sulfate and the 55mL/L being furnished with 1.5g/L, the pH controlling mixing solutions is 4-5, processes 40s, to cause the deposition of nickel metal at the temperature of 30 DEG C.
Step 8: be placed with successively by substrate in the tertiary effluent washing trough of lasting overflow and process 60s, with processing procedure liquid medicine before residual between thorough cleaning base plate line layer.
Step 9: substrate is put into chemical nickel-plating liquid (specifically forming in table 3), controlling the pH of chemical nickel-plating liquid is 4-5, at the temperature of 85 DEG C, process 20min, thus at the copper wire layer surface deposition nickel dam of substrate.
Step 10: the substrate that deposited nickel dam is placed with successively in the tertiary effluent washing trough of lasting overflow and processes 60s, processing procedure liquid medicine before residual with thorough clean plate face.
Step 11: substrate is put into chemical palladium plating solution, controlling chemical palladium plating solution pH is 7-8, processes 10min, in nickel dam surface deposition palladium layers at the temperature of 48 DEG C.
Step 12: the substrate that deposited palladium layers is placed with successively in the tertiary effluent washing trough of lasting overflow and processes 60s, processing procedure liquid medicine before residual with thorough clean plate face.
Step 13: substrate is put into chemical gold plating liquid, the pH controlling chemical gold plating liquid is 7.5-8, processes 10min, in palladium layers surface deposition layer gold at the temperature of 85 DEG C.
Step 14: the substrate that deposited layer gold is placed with successively in the tertiary effluent washing trough of lasting overflow and processes 60s, processing procedure liquid medicine before residual with thorough clean plate face.
Step 15: baking oven substrate being put into 80 DEG C dries 12min, the moisture on removing substrate.
Thus the wiring board of obtained embodiment 1-3, the character of wiring board is as shown in table 4.
Table 2
Table 3
Comparative example 1
Method according to embodiment 1 manufactures wiring board, and difference is, not containing ammoniacal liquor in the micro-etching agent in step 3, thus obtained wiring board.The character of wiring board is as shown in table 4.
Comparative example 2
Method according to embodiment 1 manufactures wiring board, and difference is, the pH of the micro-etching agent in step 3 is 8, thus obtained wiring board.The character of wiring board is as shown in table 4.
Embodiment 4
The present embodiment is for illustration of wiring board provided by the invention and preparation method thereof.
Method according to embodiment 1 manufactures wiring board, difference is, in micro-etching agent in step 3, the concentration of the sulfuric acid (concentration is 98 % by weight) of the first micro-etching agent is 64mL/L, the concentration of hydrogen peroxide (concentration is 30 % by weight) is 220mL/L, the concentration of the ammoniacal liquor (concentration is 25 % by weight) of the second micro-etching agent is 264mL/L, thus obtained wiring board.The character of wiring board is as shown in table 4.
Embodiment 5
The present embodiment is for illustration of wiring board provided by the invention and preparation method thereof.
Method according to embodiment 1 manufactures wiring board, difference is, in chemical nickel-plating liquid in step 9, the content of single nickel salt is 52g/L, the content of sodium hypophosphite is 55g/L, and the content of Trisodium Citrate is 49g/L, and the content of sodium-acetate is 12g/L, the content of thiocarbamide is 1.4mg/L, thus obtained wiring board.The character of wiring board is as shown in table 4.
Embodiment 6
Method according to embodiment 1 manufactures wiring board, and difference is, adopts the aluminium oxide ceramic substrate of same size to replace aluminum nitride ceramic substrate, thus obtained wiring board.The character of wiring board is as shown in table 4.
Table 4
As can be seen from Table 4, between copper wire layer of the present invention and nickel dam, there is higher bonding force, and wiring board has excellent heat-sinking capability.
More than describe the preferred embodiment of the present invention in detail; but the present invention is not limited to the detail in above-mentioned embodiment, within the scope of technical conceive of the present invention; can carry out multiple simple variant to technical scheme of the present invention, these simple variant all belong to protection scope of the present invention.
It should be noted that in addition, each concrete technical characteristic described in above-mentioned embodiment, in reconcilable situation, can be combined by any suitable mode, in order to avoid unnecessary repetition, the present invention illustrates no longer separately to various possible array mode.
In addition, also can carry out arbitrary combination between various different embodiment of the present invention, as long as it is without prejudice to thought of the present invention, it should be considered as content disclosed in this invention equally.
Claims (10)
1. a micro-etching agent, described micro-etching agent comprises the first micro-etching agent component and the second micro-etching agent component, described first micro-etching agent component contains the aqueous solution of sulfuric acid and hydrogen peroxide, described second micro-etching agent component is ammoniacal liquor, and the pH value of the mixed system of described first micro-etching agent component and described second micro-etching agent component is 2-4.
2. micro-etching agent according to claim 1, wherein, in described first micro-etching agent component, the concentration of sulfuric acid is 40-120g/L, and the concentration of hydrogen peroxide is 30-75g/L; In described second micro-etching agent component, the concentration of ammoniacal liquor is 20-65g/L.
3. the manufacture method of a wiring board, described method comprises carries out microetch by the copper wire layer of micro-etching agent at least one surface being attached to ceramic substrate, and the surface of copper wire layer after microetch is formed nickel dam and optional palladium layers and layer gold, containing silver in described copper wire layer, wherein, described micro-etching agent is the micro-etching agent described in claim 1 or 2.
4. method according to claim 3, wherein, the process of described microetch comprises: after the first microetch component in described micro-etching agent and the mixing of the second microetch component, described copper wire layer contacted to carry out microetch with the mixed system of described first microetch component with described second microetch component immediately.
5. the method according to claim 3 or 4, wherein, the temperature of described microetch is 15-35 DEG C; The time of described microetch is 30-50s.
6. method according to claim 3, wherein, described ceramic substrate is aluminum nitride ceramic substrate, aluminium oxide ceramic substrate or silicon carbide ceramics substrate.
7. method according to claim 6, wherein, described ceramic substrate is aluminum nitride ceramic substrate.
8. method according to claim 3, wherein, the process forming nickel dam comprises: carry out chemical nickel plating by chemical nickel-plating liquid to the surface of copper wire layer, described chemical nickel-plating liquid contains nickel salt, reductive agent, buffer reagent, stablizer and complexing agent, and the content of described nickel salt is 12-50g/L, the content of described reductive agent is 15-50g/L, and the content of described buffer reagent is 5-20g/L, the content of described complexing agent is 25-45g/L, and the content of described stablizer is 0.5-5mg/L; The pH value of described chemical nickel-plating liquid is 3-5.
9. method according to claim 8, wherein, described reductive agent is sodium hypophosphite, and described buffer reagent is sodium-acetate, and described stablizer is thiocarbamide, and described complexing agent is Trisodium Citrate.
10. method according to claim 8 or claim 9, the temperature of described chemical nickel plating is 80-85 DEG C; The time of described chemical nickel plating is 25-35min.
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| CN201410119458.9A CN104947110A (en) | 2014-03-27 | 2014-03-27 | Micro etchant, production method of circuit board and circuit board |
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| CN201410119458.9A CN104947110A (en) | 2014-03-27 | 2014-03-27 | Micro etchant, production method of circuit board and circuit board |
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| CN105734571A (en) * | 2016-04-21 | 2016-07-06 | 广州恩源化工科技有限公司 | Metal surface micro-etching liquid |
| CN107201519A (en) * | 2017-05-18 | 2017-09-26 | 苏州晶瑞化学股份有限公司 | A kind of selective two-component etching solution of titanium |
| CN113481508A (en) * | 2021-05-26 | 2021-10-08 | 绍兴德汇半导体材料有限公司 | Etching solution and etching method for removing etching residues of ceramic substrate |
| CN115558931A (en) * | 2022-10-26 | 2023-01-03 | 广东华智芯电子科技有限公司 | Refining method of copper surface crystal flower, corrosion liquid combination and application thereof |
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| CN113481508A (en) * | 2021-05-26 | 2021-10-08 | 绍兴德汇半导体材料有限公司 | Etching solution and etching method for removing etching residues of ceramic substrate |
| CN115558931A (en) * | 2022-10-26 | 2023-01-03 | 广东华智芯电子科技有限公司 | Refining method of copper surface crystal flower, corrosion liquid combination and application thereof |
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