KR101328156B1 - Synthesis of etching agent for pcb and lcd semiconductor - Google Patents
Synthesis of etching agent for pcb and lcd semiconductor Download PDFInfo
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- KR101328156B1 KR101328156B1 KR1020120070813A KR20120070813A KR101328156B1 KR 101328156 B1 KR101328156 B1 KR 101328156B1 KR 1020120070813 A KR1020120070813 A KR 1020120070813A KR 20120070813 A KR20120070813 A KR 20120070813A KR 101328156 B1 KR101328156 B1 KR 101328156B1
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- 239000004065 semiconductor Substances 0.000 title claims abstract description 19
- 238000005530 etching Methods 0.000 title claims abstract description 7
- 230000015572 biosynthetic process Effects 0.000 title claims 3
- 238000003786 synthesis reaction Methods 0.000 title claims 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000001816 cooling Methods 0.000 claims abstract description 31
- 238000002156 mixing Methods 0.000 claims abstract description 25
- 238000001914 filtration Methods 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 22
- 230000032683 aging Effects 0.000 claims abstract description 19
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 17
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 16
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 14
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 5
- 239000000376 reactant Substances 0.000 claims description 49
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 claims description 28
- 238000002425 crystallisation Methods 0.000 claims description 21
- 230000008025 crystallization Effects 0.000 claims description 21
- 239000000243 solution Substances 0.000 claims description 15
- 239000007864 aqueous solution Substances 0.000 claims description 14
- 235000010288 sodium nitrite Nutrition 0.000 claims description 14
- 230000002194 synthesizing effect Effects 0.000 claims description 12
- VPIXQGUBUKFLRF-UHFFFAOYSA-N 3-(2-chloro-5,6-dihydrobenzo[b][1]benzazepin-11-yl)-N-methyl-1-propanamine Chemical compound C1CC2=CC=C(Cl)C=C2N(CCCNC)C2=CC=CC=C21 VPIXQGUBUKFLRF-UHFFFAOYSA-N 0.000 claims description 10
- 238000001308 synthesis method Methods 0.000 claims description 4
- HAMNKKUPIHEESI-UHFFFAOYSA-N aminoguanidine Chemical compound NNC(N)=N HAMNKKUPIHEESI-UHFFFAOYSA-N 0.000 abstract description 2
- 238000001953 recrystallisation Methods 0.000 abstract 3
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 abstract 2
- 235000010344 sodium nitrate Nutrition 0.000 abstract 1
- 239000004317 sodium nitrate Substances 0.000 abstract 1
- 230000003407 synthetizing effect Effects 0.000 abstract 1
- 239000012467 final product Substances 0.000 description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- 239000008213 purified water Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 239000000460 chlorine Substances 0.000 description 4
- 229910052801 chlorine Inorganic materials 0.000 description 4
- -1 chlorine ions Chemical class 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000005260 corrosion Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 150000004682 monohydrates Chemical class 0.000 description 3
- 239000007858 starting material Substances 0.000 description 3
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000005070 ripening Effects 0.000 description 2
- JVSMPWHQUPKRNV-UHFFFAOYSA-N 2h-tetrazol-5-amine;hydrate Chemical compound O.NC=1N=NNN=1 JVSMPWHQUPKRNV-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- LVYZJEPLMYTTGH-UHFFFAOYSA-H dialuminum chloride pentahydroxide dihydrate Chemical compound [Cl-].[Al+3].[OH-].[OH-].[Al+3].[OH-].[OH-].[OH-].O.O LVYZJEPLMYTTGH-UHFFFAOYSA-H 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000035800 maturation Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
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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
- 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
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K13/00—Etching, surface-brightening or pickling compositions
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/0011—Working of insulating substrates or insulating layers
- H05K3/0017—Etching of the substrate by chemical or physical means
- H05K3/002—Etching of the substrate by chemical or physical means by liquid chemical etching
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- Microelectronics & Electronic Packaging (AREA)
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- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
Description
본 발명은 인쇄회로기판(PCB) 및 LCD반도체용 에칭제 합성방법에 관한 것으로, 혼합단계, 첨가단계, 숙성(Aging)단계, 산도조절단계, 냉각결정화단계 및 여과건조단계로 이루어진다.
The present invention relates to a method for synthesizing an etchant for a printed circuit board (PCB) and an LCD semiconductor, and comprises a mixing step, an addition step, an aging step, an acidity control step, a cooling crystallization step, and a filtration drying step.
본 발명은 인쇄회로기판 및 LCD반도체용 에칭제 합성방법에 관한 것으로, 혼합단계, 첨가단계, 숙성단계, 산도조절단계, 냉각결정화단계 및 여과건조단계로 이루어진다.The present invention relates to a method for synthesizing the etchant for printed circuit boards and LCD semiconductors, comprising a mixing step, addition step, aging step, acidity control step, cooling crystallization step and filtration drying step.
에칭(Etching)제는 인쇄회로기판(PCB) 및 LCD반도체 등 넓은 분야의 금속 표면 처리 산업분야에서 널리 사용되고 있으며, 특히 전자 산업 분야의 부품은 고도의 정밀도를 요하게 됨에 따라 향상된 품질의 에칭제에 관한 연구개발이 절실하다.Etching agents are widely used in the metal surface treatment industry of a wide range of fields such as printed circuit boards (PCB) and LCD semiconductors, and in particular, the parts of the electronics industry require high precision and thus, R & D is urgently needed.
종래에는 사용량의 대부분을 수입하여 사용하였으며, 이에 따라 국내에서도 에칭제에 관한 기술개발의 움직임이 활발히 이루어지고 있으나, 기술부족으로 인한 여러 가지 문제점이 발생하였다. 이는 인쇄회로기판 및 LCD용 에칭제를 합성할 때 반응물질 중에 염산을 사용함으로써, 최종 제품의 생성물에서 염소이온이 검출되어 금속과의 표면 접촉 시 부식을 야기하는 문제점이 발생하였으며, 또한 제품의 다양성이 확보되지 못하여 사용자로 하여금 에칭제를 사용함에 있어서 편리성이 떨어지는 문제점이 발생하였다.
In the past, most of the amount used was imported and used, and thus, the movement of technology development regarding the etchant was actively made in Korea, but various problems occurred due to the lack of technology. This is caused by the use of hydrochloric acid in the reactants when synthesizing the etchant for printed circuit boards and LCDs, chlorine ions are detected in the product of the final product, causing a problem of corrosion on the surface contact with the metal, and also a variety of products This could not be secured, causing a problem of inconvenience for the user to use the etchant.
본 발명의 목적은 아미노구아니딘 탄산염(Aminoguanidine hicarbonate)을 출발물질로 사용하고, 반응물의 산도 조절 물질로 염산이 아닌 황산을 사용하여 염소이온이 검출되지 않는 에칭제를 제공하는 것이다.It is an object of the present invention to provide an etchant which does not detect chlorine ions using aminoguanidine hicarbonate as a starting material and sulfuric acid rather than hydrochloric acid as the acidity adjusting material of the reactants.
본 발명의 다른 목적은 최종 제품의 수율이 80%에 달하여 높은 수득률을 나타내며, 최종제품을 모노하이드레이트(monohydrate)상태로 제공하여 사용자의 용해도에 따른 편의성을 제공하는 것이다.
Another object of the present invention is to yield a high yield of the final product reaches 80%, to provide a convenience according to the solubility of the user by providing the final product in the monohydrate (monohydrate) state.
본 발명의 목적은 질산수용액과 아미노구아니딘 탄산염을 혼합하여 교반하는 혼합단계, 상기 혼합단계를 거쳐 생성된 반응물에 아질산나트륨 수용액을 첨가하는 첨가단계, 상기 첨가단계를 통해 생성된 반응물에 암모니아를 투입하고 가열하여 반응물을 숙성시키는 숙성단계, 상기 숙성단계를 거쳐 생성된 반응물을 냉각하고 황산을 첨가하여 반응물의 산도를 조절하는 산도조절단계, 상기 산도조절단계를 거쳐 생성된 반응물을 냉각시켜 결정화하는 냉각결정화단계 및 상기 냉각결정화단계를 통해 생성된 반응물을 여과하고 건조시키는 여과건조단계로 이루어지는 것을 특징으로 하는 인쇄회로기판 및 LCD반도체용 에칭제의 합성방법을 제공함에 의해 달성된다.An object of the present invention is a mixing step of mixing and stirring the aqueous solution of nitric acid and aminoguanidine carbonate, the addition step of adding an aqueous sodium nitrite solution to the reaction product produced through the mixing step, and ammonia is added to the reaction product produced through the addition step Aging step of aging the reactants by heating, cooling the reactants produced through the aging step, acidity adjusting step of adjusting the acidity of the reactants by adding sulfuric acid, cooling crystallization to cool the crystallization produced through the acidity adjusting step It is achieved by providing a method for synthesizing the etchant for printed circuit boards and LCD semiconductors, characterized in that it comprises a filtration and drying step of filtering and drying the reactants produced by the cooling crystallization step.
본 발명의 바람직한 특징에 따르면, 상기 혼합단계는 질산수용액과 아미노구아니딘 탄산염을 5 내지 30℃의 온도에서 투입하고 교반하여 이루어지는 것으로 한다.According to a preferred feature of the invention, the mixing step is to be made by adding and stirring the aqueous nitric acid solution and aminoguanidine carbonate at a temperature of 5 to 30 ℃.
본 발명의 더 바람직한 특징에 따르면, 상기 첨가단계는 상기 혼합단계를 거쳐 생성된 5 내지 30℃의 반응물에 아질산나트륨 수용액을 첨가하여 이루어지며, 상기 아질산나트륨 수용액은 1 내지 5시간 동안 질산수용액 100 중량부 대비 40 내지 70 중량부를 투입하여 이루어지는 것으로 한다.
According to a more preferred feature of the invention, the addition step is made by adding an aqueous sodium nitrite solution to the reaction product of 5 to 30 ℃ produced through the mixing step, the sodium nitrite aqueous solution is 100 weight of aqueous nitric acid solution for 1 to 5 hours 40 to 70 parts by weight relative to the part is assumed to be made.
본 발명의 더욱 바람직한 특징에 따르면, 상기 숙성단계는 상기 첨가단계를 통해 생성된 반응물에 암모니아를 투입하고 가열하여 90 내지 120℃의 온도에서 1 내지 5시간 동안 반응물을 숙성시키는 것을 특징으로 이루어진다.According to a more preferable feature of the present invention, the aging step is characterized in that the ammonia is added to the reactants produced through the addition step and heated to mature the reactants for 1 to 5 hours at a temperature of 90 to 120 ℃.
본 발명의 더욱 더 바람직한 특징에 따르면, 상기 산도조절단계는 상기 숙성단계를 거쳐 생성된 반응물을 30 내지 80℃의 온도로 냉각시키고, 황산을 투입하여 반응물의 산도(pH)를 2 내지 6으로 조절하여 이루어지는 것으로 한다.According to an even more preferred feature of the present invention, the acidity control step is to cool the reactants produced through the aging step to a temperature of 30 to 80 ℃, sulfuric acid is added to adjust the acidity (pH) of the reactants to 2 to 6 It shall be made by.
본 발명의 더욱 더 바람직한 특징에 따르면, 상기 냉각결정화단계는 상기 산도조절단계를 거쳐 생성된 반응물을 1 내지 20℃의 온도로 냉각하고 결정화하여 이루어지는 것으로 한다.According to a further preferred feature of the present invention, the cooling crystallization step is to be made by cooling and crystallizing the reactants produced through the acidity control step to a temperature of 1 to 20 ℃.
본 발명의 더욱 더 바람직한 특징에 따르면, 상기 여과건조단계는 상기 냉각결정화단계를 통해 생성된 반응물을 여과장치를 통해 여과한 후, 50 내지 70℃ 온도의 건조기에서 1 내지 3시간 동안 건조시켜 이루어지는 것으로 한다.
According to a further preferred feature of the present invention, the filtration drying step is to be made by filtering the reactants produced through the cooling crystallization step through a filtration device, and then dried for 1 to 3 hours in a dryer of 50 to 70 ℃ temperature do.
본 발명에 따른 인쇄회로기판(PCB) 및 LCD반도체용 에칭제 합성방법은 아미노구아니딘 탄산염을 출발물질로 사용하고, 반응물의 산도 조절 물질로 염산이 아닌 황산을 사용하여 염소이온이 검출되지 않는 에칭제를 제공함으로써, 금속 표면과의 접촉시 부식을 방지하는데 있어서 탁월한 효과를 나타낸다.In the method for synthesizing the etchant for printed circuit boards (PCBs) and LCD semiconductors according to the present invention, an etchant which does not detect chlorine ions using aminoguanidine carbonate as a starting material and sulfuric acid rather than hydrochloric acid as an acidity controlling material of the reactants By providing a superior effect in preventing corrosion upon contact with metal surfaces.
또한, 본 발명에 따른 에칭제 합성방법은 최종 제품의 수율이 80%에 달하여 높은 수득률을 나타내며, 최종제품을 모노하이드레이트(monohydrate)상태로 제공하여 사용자의 용해도에 따른 편의성을 제공할 수 있는 이점을 나타낸다.
In addition, the etchant synthesis method according to the present invention has a high yield of 80% yield of the final product, and provides the final product in the monohydrate (monohydrate) state to provide the convenience according to the solubility of the user Indicates.
도 1은 본 발명에 따른 인쇄회로기판 및 LCD반도체용 에칭제 합성방법을 나타낸 순서도이다.1 is a flowchart illustrating a method for synthesizing an etchant for a printed circuit board and an LCD semiconductor according to the present invention.
이하에는, 본 발명의 바람직한 실시예와 각 성분의 물성을 상세하게 설명하되, 이는 본 발명이 속하는 기술분야에서 통상의 지식을 가진 자가 발명을 용이하게 실시할 수 있을 정도로 상세하게 설명하기 위한 것이지, 이로 인해 본 발명의 기술적인 사상 및 범주가 한정되는 것을 의미하지는 않는다.
Hereinafter, preferred embodiments of the present invention and physical properties of the respective components will be described in detail with reference to the accompanying drawings. However, the present invention is not limited thereto, And this does not mean that the technical idea and scope of the present invention are limited.
본 발명에 따른 인쇄회로기판 및 LCD반도체용 에칭제의 합성방법은 질산수용액과 아미노구아니딘 탄산염을 혼합하여 교반하는 혼합단계(S101), 상기 혼합단계(S101)를 거쳐 생성된 반응물에 아질산나트륨 수용액을 첨가하는 첨가단계(S103), 상기 첨가단계(S103)를 통해 생성된 반응물에 암모니아를 투입하고 가열하여 반응물을 숙성시키는 숙성단계(S105), 상기 숙성단계(S105)를 거쳐 생성된 반응물을 냉각하고 황산을 첨가하여 반응물의 산도를 조절하는 산도조절단계(S107), 상기 산도조절단계(S107)를 거쳐 생성된 반응물을 냉각시켜 결정화하는 냉각결정화단계(S109) 및 상기 냉각결정화단계(S109)를 통해 생성된 반응물을 여과하고 건조시키는 여과건조단계(S111)로 이루어진다.
Synthesis method of the etchant for printed circuit board and LCD semiconductor according to the present invention is a sodium nitrite aqueous solution to the reactants produced through the mixing step (S101), the mixing step (S101) by mixing and stirring the aqueous solution of nitric acid and amino guanidine carbonate Addition step (S103) to add, adding ammonia to the reactants produced through the addition step (S103) and the maturation step (S105) to mature the reactants by heating, and cooling the reactants generated through the aging step (S105) and Acidity adjustment step (S107) of controlling the acidity of the reactants by adding sulfuric acid, through the crystallization step (S109) and the cooling crystallization step (S109) of the crystallization by cooling the reactants generated through the acidity control step (S107) It consists of a filtration drying step (S111) for filtering and drying the resulting reactants.
전술한 혼합단계(S101)는 질산수용액과 아미노구아니딘 탄산염을 혼합하여 교반하는 혼합단계(S101)로, 정제수와 질산을 1:1 내지 5:1 중량부 비율로 혼합한 질산수용액을 제조하여 100 중량부를 투입하고, 질산수용액 100 중량부 대비 아미노구아니딘 탄산염 20 내지 50 중량부를 투입하여 5 내지 30℃의 온도에서 10 내지 50분 동안 교반하여 이루어진다.
The mixing step (S101) is a mixing step (S101) of mixing and stirring an aqueous solution of nitric acid and aminoguanidine carbonate, and preparing an aqueous solution of nitric acid mixed with purified water and nitric acid at a ratio of 1: 1 to 5: 1 parts by weight to 100 wt%. A part is added, and 20 to 50 parts by weight of aminoguanidine carbonate is added to 100 parts by weight of aqueous nitric acid solution, followed by stirring at a temperature of 5 to 30 ° C. for 10 to 50 minutes.
전술한 첨가단계(S103)는 상기 혼합단계(S101)를 거쳐 생성된 5 내지 30℃의 반응물에 아질산나트륨 수용액을 첨가하여 이루어지며, 아질산나트륨 수용액은 1 내지 5시간 동안 질산수용액 100 중량부 대비 40 내지 70 중량부를 투입하여 이루어진다. 상기 아질산나트륨 수용액은 정제수와 아질산나트륨을 1:1 내지 5:1 중량부 비율로 혼합하여 이루어진다.
The above-described addition step (S103) is made by adding an aqueous sodium nitrite solution to the reaction product of 5 to 30 ℃ produced through the mixing step (S101), the sodium nitrite aqueous solution is 40 to 100 parts by weight of aqueous solution of nitric acid for 1 to 5 hours To 70 parts by weight. The sodium nitrite aqueous solution is made by mixing purified water and sodium nitrite in a ratio of 1: 1 to 5: 1 parts by weight.
전술한 숙성단계(S105)는 상기 첨가단계(S103)를 통해 생성된 반응물에 암모니아를 투입하고 가열하여 반응물을 숙성시키는 숙성단계로, 상기 첨가단계(S103)를 통해 생성된 반응물에 질산수용액 100 중량부 대비 암모니아 20 내지 50 중량부를 투입한 후 가열하여 온도를 상승시킨다. 90 내지 120℃의 온도까지 가열하여 반응물의 온도를 상승시킨 후, 상기 온도를 유지하면서 1 내지 5시간 동안 반응물을 숙성시킨다.
The above-described aging step (S105) is a ripening step of aging the reactants by adding ammonia to the reactants generated through the addition step (S103) and heating, 100 weight of aqueous nitric acid solution to the reactants generated through the addition step (S103) 20 to 50 parts by weight of ammonia relative to the amount is added and heated to increase the temperature. After heating to a temperature of 90 to 120 ℃ to raise the temperature of the reactants, the reactants are aged for 1 to 5 hours while maintaining the temperature.
전술한 산도조절단계(S107)는 상기 숙성단계(S105)를 거쳐 생성된 반응물을 냉각하고 황산을 첨가하여 반응물의 산도를 조절하는 산도조절단계(S107)로, 상기 숙성단계(S105)를 거쳐 생성된 반응물을 30 내지 80℃의 온도로 냉각시킨 후, 황산을 투입하여 반응물의 산도를 조절한다. 이때 황산은 정제수와 1:1 내지 1:5 중량부 비율로 혼합하여 황산수용액으로 제조하여 질산수용액 100 중량부 대비 150 내지 200 중량부를 투입하며, 생성물의 산도(pH)는 2 내지 6으로 조절한다.
The above-described acidity control step (S107) is an acidity control step (S107) for cooling the reactants produced through the aging step (S105) and adding the sulfuric acid to adjust the acidity of the reactants, generated through the aging step (S105). After cooling the reactant to a temperature of 30 to 80 ℃, sulfuric acid is added to adjust the acidity of the reactant. In this case, sulfuric acid is mixed with purified water at a ratio of 1: 1 to 1: 5 parts by weight to prepare a sulfuric acid solution, and 150 to 200 parts by weight based on 100 parts by weight of nitric acid solution, and the acidity (pH) of the product is adjusted to 2 to 6. .
전술한 냉각결정화단계(S109)는 상기 산도조절단계(S107)를 거쳐 생성된 반응물을 냉각하고 결정화하는 냉각결정화단계(S109)로, 상기 산도조절단계(S107)를 거쳐 생성된 반응물을 1 내지 30℃의 온도로 냉각시킨 후, 1 내지 20℃ 온도의 냉장실에서 1 내지 7시간 동안 냉장보관하여 결정화한다.
The above-described cooling crystallization step (S109) is a cooling crystallization step (S109) of cooling and crystallizing the reactants generated through the acidity adjusting step (S107), and the reactants produced through the acidity adjusting step (S107) 1 to 30. After cooling to a temperature of ℃, it is refrigerated for 1 to 7 hours in a refrigerating chamber at a temperature of 1 to 20 ℃ crystallization.
전술한 여과건조단계(S111)는 상기 냉각결정화단계(S109)를 통해 생성된 반응물을 여과하고 건조시키는 여과건조단계(S111)로, 상기 냉각결정화단계(S109)를 통해 생성된 반응물을 여과장치를 통해 여과한 후, 50 내지 70℃ 온도의 건조기에서 1 내지 3시간 동안 공기를 주입하며 건조시켜 모노하이드레이트(monohydrate)상태의 최종 생성물을 얻는다.
The above-mentioned filtration drying step (S111) is a filtration drying step (S111) for filtering and drying the reactants produced through the cooling crystallization step (S109), and filtering the reactants generated through the cooling crystallization step (S109). After filtering through, the resultant product was dried by injecting air for 1 to 3 hours in a dryer at a temperature of 50 to 70 ° C. to obtain a monohydrate final product.
이하에는, 본 발명에 따른 인쇄회로기판(PCB) 및 LCD반도체용 에칭제 합성방법을 실시예를 들어 설명한다.
Hereinafter, a method for synthesizing a printed circuit board (PCB) and an etchant for an LCD semiconductor according to the present invention will be described.
<실시예1>≪ Example 1 >
4-neck 3L 플라스크 반응기에 질산(순도69%) 204g과 정제수 253g이 혼합된 질산수용액을 투입하고, 아미노구아니딘 탄산염 155g을 투입하여, 15℃의 온도에서 30분간 교반한다. 상기 혼합물에 아질산나트륨(순도97%) 71.1g과 정제수 166g을 혼합한 아질산나트륨 수용액을 3시간에 걸쳐서 천천히 투입하도록 한다. 이때 온도는 10 내지 15℃를 유지하도록 한다. 아질산나트륨 수용액의 투입이 끝난 후, 20℃에서 1시간 동안 반응물을 교반하여 숙성시킨다. 상기 혼합물에 암모니아(순도28%) 144g을 한꺼번에 전량을 투입하고 가열하여 온도를 103℃로 상승시킨 후, 103℃에 도달하면 교반하여 3시간 동안 숙성시킨다. 숙성과정을 마친 반응물의 온도를 50℃로 냉각시킨 후, 황산(순도98%) 235g과 정제수 576g을 혼합한 황산 수용액을 제조하여, 반응물에 황산 수용액을 투입하면서 산도(pH)를 4로 조절한다. 산도를 조절한 반응물은 10℃로 냉각시켜 5시간 동안 냉장보관하여 결정화한다. 결정 상태의 반응물은 여과 과정을 거친 후, 공기를 주입하며 60℃의 건조기에서 2시간 동안 건조시켜 최종 생성물인 5-아미노테트라졸 모노하이드레이트(5-aminotetrazole monohydrate)를 얻는다.
Into a 4-neck 3L flask reactor was added an aqueous nitrate solution in which 204 g of nitric acid (69% purity) and 253 g of purified water were mixed, 155 g of aminoguanidine carbonate was added, and stirred at a temperature of 15 ° C for 30 minutes. To the mixture was slowly added sodium nitrite aqueous solution mixed with 71.1 g of sodium nitrite (purity 97%) and 166 g of purified water over 3 hours. At this time, the temperature is maintained at 10 to 15 ℃. After the addition of the aqueous sodium nitrite solution, the reaction mass was aged for 1 hour at 20 ° C. The mixture was added with a total amount of 144 g of ammonia (28% purity) at once and heated to raise the temperature to 103 ° C., and then stirred to reach 103 ° C. to mature for 3 hours. After the temperature of the reactant is aged to 50 ° C, an aqueous sulfuric acid solution is prepared in which 235 g of sulfuric acid (98% purity) and 576 g of purified water are mixed. The pH (pH) is adjusted to 4 while adding an aqueous sulfuric acid solution to the reaction product. . The acidity-controlled reactant is cooled to 10 ℃ and refrigerated for 5 hours to crystallize. The reactant in the crystalline state is filtered and then air-dried and dried in a dryer at 60 ° C. for 2 hours to obtain 5-aminotetrazole monohydrate, the final product.
<실시예2>≪ Example 2 >
상기 실시예 1와 동일하게 실시하되, 최종 생성물의 질량을 측정하여 수득률을 계산한다.The same procedure as in Example 1 was carried out, but the yield was calculated by measuring the mass of the final product.
<실시예3>≪ Example 3 >
상기 실시예 1와 동일하게 실시하되, 최종 생성물의 질량을 측정하여 수득률을 계산한다.The same procedure as in Example 1 was carried out, but the yield was calculated by measuring the mass of the final product.
<실시예4><Example 4>
상기 실시예 1와 동일하게 실시하되, 최종 생성물의 질량을 측정하여 수득률을 계산한다.The same procedure as in Example 1 was carried out, but the yield was calculated by measuring the mass of the final product.
<실시예5>≪ Example 5 >
상기 실시예 1와 동일하게 실시하되, 최종 생성물의 질량을 측정하여 수득률을 계산한다.
The same procedure as in Example 1 was carried out, but the yield was calculated by measuring the mass of the final product.
전술한 실시예 1 내지 5를 통해 제조된 인쇄회로기판(PCB) 및 LCD반도체용 에칭제 합성방법에 의한 최종 제품의 수득률을 계산하여 아래 표 1에 나타내었다. The yield of the final product by the method of synthesizing the printed circuit board (PCB) and the etchant for LCD semiconductors prepared through the above Examples 1 to 5 is calculated and shown in Table 1 below.
<표 1>TABLE 1
상기 표 1에서 보는 바와 같이, 실시예 1 내지 5를 통해 생성된 최종 생성물의 질량을 측정하여 최종 제품의 수득률을 계산한 결과를 살펴보면 평균 80.2%의 높은 수득률을 나타냄을 알 수 있다.
As shown in Table 1, the results of calculating the yield of the final product by measuring the mass of the final product produced through Examples 1 to 5 can be seen that the average yield of 80.2%.
따라서, 본 발명에 따른 인쇄회로기판(PCB) 및 LCD반도체용 에칭제 합성방법은 최종 제품의 수율이 80%에 달하여 높은 수득률을 나타내며, 최종제품을 모노하이드레이트(monohydrate)상태로 제공하여 사용자의 용해도에 따른 편의성을 제공할 수 있는 이점을 나타낸다.Therefore, the method for synthesizing the etchant for printed circuit board (PCB) and LCD semiconductor according to the present invention shows a high yield with the yield of the final product reaches 80%, and provides the final product in the monohydrate state (monohydrate) solubility of the user Represents an advantage that can provide convenience according to.
또한, 아미노구아니딘 탄산염을 출발물질로 사용하고, 반응물의 산도 조절 물질로 염산이 아닌 황산을 사용하여 염소이온이 검출되지 않는 에칭제를 제공함으로써, 금속 표면과의 접촉시 부식을 방지하는데 있어서 탁월한 효과를 나타낸다.
In addition, by using aminoguanidine carbonate as a starting material and sulfuric acid rather than hydrochloric acid as the acidity adjusting material of the reactants, an etching agent which does not detect chlorine ions is excellent in preventing corrosion on contact with metal surfaces. Indicates.
S101 ; 혼합단계
S103 ; 첨가단계
S105 ; 숙성단계
S107 ; 산도조절단계
S109 ; 냉각결정화단계
S111 ; 여과건조단계S101; Mixing step
S103; Addition step
S105; Ripening step
S107; PH control stage
S109; Cooling Crystallization Step
S111; Filtration drying step
Claims (7)
상기 혼합단계를 거쳐 생성된 반응물에 아질산나트륨 수용액을 첨가하는 첨가단계;
상기 첨가단계를 통해 생성된 반응물에 암모니아를 투입하고 가열하여 반응물을 숙성시키는 숙성단계;
상기 숙성단계를 거쳐 생성된 반응물을 냉각하고 황산을 첨가하여 반응물의 산도를 조절하는 산도조절단계;
상기 산도조절단계를 거쳐 생성된 반응물을 냉각시켜 결정화하는 냉각결정화단계; 및
상기 냉각결정화단계를 통해 생성된 반응물을 여과하고 건조시키는 여과건조단계;로 이루어지는 것을 특징으로 하는 인쇄회로기판 및 LCD반도체용 에칭제의 합성방법.
A mixing step of mixing and stirring the aqueous nitric acid solution and aminoguanidine carbonate;
An addition step of adding an aqueous sodium nitrite solution to the reaction product produced through the mixing step;
Aging step of adding ammonia to the reactants produced through the addition step and heating to mature the reactants;
An acidity adjustment step of controlling the acidity of the reactants by cooling the reactants generated through the aging step and adding sulfuric acid;
A cooling crystallization step of crystallizing the reactants generated through the acidity adjusting step; And
Filtration drying step of filtering and drying the reactants produced by the cooling crystallization step; Synthesizing method for a printed circuit board and an LCD semiconductor.
상기 혼합단계는 질산수용액과 아미노구아니딘 탄산염을 5 내지 30℃의 온도에서 투입하고 교반하는 것을 특징으로 하는 인쇄회로기판 및 LCD반도체용 에칭제의 합성방법.
The method according to claim 1,
The mixing step is a method of synthesizing the etchant for printed circuit board and LCD semiconductor, characterized in that the aqueous solution of nitric acid and amino guanidine carbonate at a temperature of 5 to 30 ℃.
상기 첨가단계는 상기 혼합단계를 거쳐 생성된 5 내지 30℃의 반응물에 아질산나트륨 수용액을 첨가하여 이루어지며, 상기 아질산나트륨 수용액은 1 내지 5시간 동안 질산수용액 100 중량부 대비 40 내지 70 중량부를 투입하는 것을 특징으로 하는 인쇄회로기판 및 LCD반도체용 에칭제의 합성방법.
The method according to claim 1,
The addition step is made by adding a sodium nitrite aqueous solution to the reaction product of 5 to 30 ℃ produced through the mixing step, the sodium nitrite aqueous solution is added to 40 to 70 parts by weight relative to 100 parts by weight of aqueous solution of nitric acid for 1 to 5 hours A method for synthesizing an etchant for printed circuit boards and LCD semiconductors, characterized in that the.
상기 숙성단계는 상기 첨가단계를 통해 생성된 반응물에 암모니아를 투입하고 가열하여 90 내지 120℃의 온도에서 1 내지 5시간 동안 반응물을 숙성시키는 것을 특징으로 하는 인쇄회로기판 및 LCD반도체용 에칭제의 합성방법.
The method according to claim 1,
The aging step is the synthesis of the etchant for printed circuit board and LCD semiconductor, characterized in that by adding ammonia to the reactants produced through the addition step and heating to mature the reactants for 1 to 5 hours at a temperature of 90 to 120 ℃. Way.
상기 산도조절단계는 상기 숙성단계를 거쳐 생성된 반응물을 30 내지 80℃의 온도로 냉각시키고, 황산을 투입하여 반응물의 산도(pH)를 2 내지 6으로 조절하는 것을 특징으로 하는 인쇄회로기판 및 LCD반도체용 에칭제의 합성방법.
The method according to claim 1,
The acidity adjusting step is a printed circuit board and LCD, characterized in that the reactants generated through the aging step to cool to a temperature of 30 to 80 ℃, sulfuric acid is added to adjust the acidity (pH) of the reactants to 2 to 6 Synthesis method of semiconductor etchant.
상기 냉각결정화단계는 상기 산도조절단계를 거쳐 생성된 반응물을 1 내지 20℃의 온도로 냉각시켜 결정화하는 것을 특징으로 하는 인쇄회로기판 및 LCD반도체용 에칭제의 합성방법.
The method according to claim 1,
The cooling crystallization step is a synthesis method of the etching agent for a printed circuit board and LCD semiconductor, characterized in that the crystallization by cooling the reactants produced through the acidity control step to a temperature of 1 to 20 ℃.
상기 여과건조단계는 상기 냉각결정화단계를 통해 생성된 반응물을 여과장치를 통해 여과한 후, 50 내지 70℃ 온도의 건조기에서 1 내지 3시간 동안 건조시키는 것을 특징으로 하는 인쇄회로기판 및 LCD반도체용 에칭제의 합성방법.
The method according to claim 1,
The filtration drying step is to filter the reactants produced through the cooling crystallization step through a filtration apparatus, and then etching for 1 to 3 hours in a dryer of 50 to 70 ℃ temperature etching for printed circuit boards and LCD semiconductors Synthesis of Agents.
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| KR20110115524A (en) * | 2010-04-15 | 2011-10-21 | 후지필름 가부시키가이샤 | Method for cleaning semiconductor substrate, and two-component cleaning agent for semiconductor substrate |
| KR20120044263A (en) * | 2010-10-27 | 2012-05-07 | 후지필름 가부시키가이샤 | Multi-agent type cleaning kit for semiconductor substrates, cleaning method using the same and method of producing semiconductor element |
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| KR20110115524A (en) * | 2010-04-15 | 2011-10-21 | 후지필름 가부시키가이샤 | Method for cleaning semiconductor substrate, and two-component cleaning agent for semiconductor substrate |
| KR20120044263A (en) * | 2010-10-27 | 2012-05-07 | 후지필름 가부시키가이샤 | Multi-agent type cleaning kit for semiconductor substrates, cleaning method using the same and method of producing semiconductor element |
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