CN102212804A - Alkali chemical plating solution and solution plating method thereof on silicon chip - Google Patents
Alkali chemical plating solution and solution plating method thereof on silicon chip Download PDFInfo
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- CN102212804A CN102212804A CN 201110139693 CN201110139693A CN102212804A CN 102212804 A CN102212804 A CN 102212804A CN 201110139693 CN201110139693 CN 201110139693 CN 201110139693 A CN201110139693 A CN 201110139693A CN 102212804 A CN102212804 A CN 102212804A
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Abstract
The invention discloses alkali chemical plating solution and solution plating method thereof on a silicon chip, belongs to the field of chemical industry, and relates to a method for chemically plating nickel on a silicon chip. The invention aims to provide the alkali chemical plating solution plated on the silicon chip directly by using a chemical deposition method without pretreatment and the solution plating method thereof on the silicon chip. The formula of the plating solution comprises a main salt, a buffer agent, a complexing agent, a reducing agent and a stabilizing agent. The alkali plating solution with stability, good bonding force of a coating and high plating speed is obtained by a series of research on direct nickel plating on the silicon at an intermediate temperature; and the stability of the plating solution, the bonding force of the coating and the plating speed are taken into comprehensive consideration. By the provided alkali solution plating method, the complex pretreatment problem of plating the nickel on the silicon chip is solved, and pretreatment-free nickel plating is realized.
Description
Technical field
The invention belongs to chemical field, relate to the method for chemical nickel plating on the silicon chip.
Background technology
The preparation of semiconductor silicon surface-functional metallic film is an extremely important process in many high-tech sectors, is widely used in many fields such as manufacturing, solar cell, MEMS (micro electro mechanical system) (MEMS), thin film magnetic recording material, solid-state illumination of unicircuit and semiconducter device.
Electroless plating is the important method that forms functional film.Because silicon is non-catalytic surface, so need carry out the pre-treatment process with chemical deposition at the silicon face depositing metal films, makes silicon face present the activity of electroless plating.At present, pre-treating process commonly used both at home and abroad has: form Seed Layer, palladium metal be adsorbed on strong corrosive materials such as silicon face, employing hydrofluoric acid with sensitization and activatory method silicon face is corroded activation etc. with evaporation or sputtering method.These treatment processs are because existence and the corrosive ununiformity and the excessive corrosion of active layer or Seed Layer, may influence or change the performance of silicon matrix, perhaps influence the ohmic contact between metallic film and the silicon, thereby reduce the normal use properties of functional metallic film on the silicon.
Bhansali etc. adopt ion implantation method to form the conductive thin metal layer of one deck earlier as Seed Layer at silicon face, are that electroplate on the basis with this layer Seed Layer then, form metallic film.Also the someone adopts the method for Pd etc. in the silicon face printing to make its metallization, and then electroplates the formation metallic film.In recent years, the someone attempts adopting HF etc. that silicon face is corroded activation treatment, directly carries out chemical nickel plating then on silicon, makes silicon face form the film of metallic nickel.Because when employing HF etc. carried out deep-etching, depth of corrosion and homogeneity were difficult to control, make that the reliability and stability of technology are very poor.And such method complexity, cost height, be unfavorable for some big area and require the field of delicate execution, as solar cell etc.
Summary of the invention
The purpose of this invention is to provide on a kind of silicon chip that need not pre-treatment directly utilizes chemical deposition to carry out the alkali electroless plating bath of plating bath and the plating bath method on silicon chip thereof.
The weight part that the present invention forms electroplate liquid formulation is:
Main salt: single nickel salt 25.0～30.0
Buffer reagent: ammonium chloride 20～40
Complexing agent: citric acid 50～80
Reductive agent: inferior sodium phosphate 8.0～12.0
Stablizer: sodium lauryl sulphate 0.003～0.005.
The compound method of alkali electroless plating bath of the present invention is:
A, single nickel salt, inferior sodium phosphate, citric acid, ammonium chloride, sodium lauryl sulphate are used the deionized water stirring and dissolving respectively, again citric acid, ammonium chloride, sodium lauryl sulphate are mixed;
B, with consoluet nickel salt solution, under constantly stirring, pour into and contain in the complex compound a mixing solutions in step;
C, general be consoluet sodium hypophosphite solution, under agitation, pours into by in the b solution in step;
D, the pH value conditioning agent that oneself dissolving is got well add while stirring by in the c solution in step, promptly obtain plating bath.
The plating bath method of alkali electroless plating bath of the present invention on silicon chip is: silicon chip is immersed in the plating bath fully, is plating under 60 ℃.
The present invention on the silicon under the medium temperature condition directly nickel plating carried out a series of research, obtained bath stability, binding force of cladding material better, plating speed alkali plating solution faster, take all factors into consideration bath stability, binding force of cladding material and plating speed.
The alkali plating solution method that proposes has solved the pre-treatment problem of silicon chip nickel plating complexity, has realized need not the nickel plating of pre-treatment.
Description of drawings
Fig. 1 is the sem photograph of the embodiment of the invention 1 nickel plating silicon chip surface;
Fig. 2 is the sem photograph of the embodiment of the invention 2 nickel plating silicon chip surfaces;
Fig. 3 is the sem photograph of the embodiment of the invention 3 nickel plating silicon chip surfaces;
Fig. 4 is the sem photograph of the embodiment of the invention 4 nickel plating silicon chip surfaces;
Fig. 5 is the sem photograph of the embodiment of the invention 5 nickel plating silicon chip surfaces;
Fig. 6 is the sem photograph of the embodiment of the invention 6 nickel plating silicon chip surfaces;
Fig. 7 is the sem photograph of the embodiment of the invention 7 nickel plating silicon chip surfaces;
Fig. 8 is the sem photograph of the embodiment of the invention 8 nickel plating silicon chip surfaces;
Fig. 9 is the sem photograph of the embodiment of the invention 9 nickel plating silicon chip surfaces.
Embodiment
The weight part that the present invention forms electroplate liquid formulation is:
Main salt: single nickel salt 25.0～30.0
Buffer reagent: ammonium chloride 20～40
Complexing agent: citric acid 50～80
Reductive agent: inferior sodium phosphate 8.0～12.0
Stablizer: sodium lauryl sulphate 0.003～0.005.
The compound method of alkali electroless plating bath of the present invention is:
A, single nickel salt, inferior sodium phosphate, citric acid, ammonium chloride, sodium lauryl sulphate are used the deionized water stirring and dissolving respectively, again citric acid, ammonium chloride, sodium lauryl sulphate are mixed;
B, with consoluet nickel salt solution, under constantly stirring, pour into and contain in the complex compound a mixing solutions in step;
C, general be consoluet sodium hypophosphite solution, under agitation, pours into by in the b solution in step;
D, the pH value conditioning agent that oneself dissolving is got well add while stirring by in the c solution in step, promptly obtain plating bath.
The plating bath method of alkali electroless plating bath of the present invention on silicon chip is: silicon chip is immersed in the plating bath fully, is plating under 60 ℃.
Below further detailed description to the present invention:
At first the simple clean surface of the most handy washing powder of silicon chip is washed with tap water, and distilled water flushing is put into the plating bath of stirring then, is plating under 60 ℃, though plating bath has black nickel to separate out, plating bath is undecomposed, and binding force of cladding material is general.
The preparation of plating bath: single nickel salt 25.0g/L, inferior sodium phosphate 8.0g/L, citric acid 50g/L, ammonium chloride 30.0g/L, sodium lauryl sulphate 0.005g/L.
The compound method of plating bath is: following all is to carry out at normal temperatures, and all churning time are all at 3～5 minutes
1. take by weighing single nickel salt, inferior sodium phosphate, citric acid, ammonium chloride, sodium lauryl sulphate by above-mentioned prescription and use the deionized water stirring and dissolving respectively, all every kind of amount of substances that every liter of deionized water need be put in the prescription, and will be by the good citric acid of deionized water dissolving, ammonium chloride, sodium lauryl sulphate remix;
2. with consoluet nickel salt solution, under constantly stirring, pour into and contain in the solution that 1. complex compound go on foot;
3. incite somebody to action consoluet sodium hypophosphite solution, under agitation, pour into by in the solution 2.;
4. with the good pH value conditioning agent of oneself dissolving, the pH value conditioning agent adopts the sulfuric acid of 5%NaOH solution or 10%, adds while stirring in the solution by 3. configuration, and surveying the pH value simultaneously is 9.0.
Embodiment 2
At first the simple clean surface of the most handy washing powder of silicon chip is washed with tap water, and distilled water flushing is put into the plating bath of stirring then, is plating under 60 ℃, and bath stability improves greatly, no longer includes nickel and separates out, and the bonding force of coating and silicon chip is good.
The preparation of plating bath: single nickel salt 25.0g/L, inferior sodium phosphate 8.0g/L, citric acid 70g/L, ammonium chloride 30.0g/L, sodium lauryl sulphate 0.005g/L.
The compound method of plating bath is identical with embodiment 1.
Embodiment 3
At first the simple clean surface of the most handy washing powder of silicon chip is washed with tap water, and distilled water flushing is put into the plating bath of stirring then, is plating under 60 ℃, and plating bath clarification nothing is separated out, and bonding force is general.
The preparation of plating bath: single nickel salt 25.0g/L, inferior sodium phosphate 8.0g/L, citric acid 80g/L, ammonium chloride 30.0g/L, sodium lauryl sulphate 0.005g/L.
The compound method of plating bath is identical with embodiment 1.
Embodiment 4
At first the simple clean surface of the most handy washing powder of silicon chip is washed with tap water, and distilled water flushing is put into the plating bath of stirring then, is plating under 60 ℃, and plating bath is not very stable, separate out with nickel, but binding force of cladding material is fine.
The preparation of plating bath: single nickel salt 27.0g/L, inferior sodium phosphate 10.0g/L, citric acid 70g/L, ammonium chloride 20.0g/L, sodium lauryl sulphate 0.004g/L.
The compound method of plating bath is identical with embodiment 1.
Embodiment 5
At first the simple clean surface of the most handy washing powder of silicon chip is washed with tap water, and distilled water flushing is put into the plating bath of stirring then, is plating under 60 ℃, and plating bath clarifies but bonding force is general.
The preparation of plating bath: single nickel salt 30.0g/L, inferior sodium phosphate 12.0g/L, citric acid 70g/L, ammonium chloride 40.0g/L, sodium lauryl sulphate 0.005g/L.
The compound method of plating bath is identical with embodiment 1.
Embodiment 6
At first the simple clean surface of the most handy washing powder of silicon chip is washed with tap water, and distilled water flushing is put into the plating bath of stirring then, is plating under 50 ℃, and reaction is not carried out.
The preparation of plating bath: single nickel salt 25.0g/L, inferior sodium phosphate 8.0g/L, citric acid 70g/L, ammonium chloride 30.0g/L, sodium lauryl sulphate 0.003g/L.
The compound method of plating bath is identical with embodiment 1.
Embodiment 7
At first the simple clean surface of the most handy washing powder of silicon chip is washed with tap water, then distilled water flushing, putting into the plating bath of stirring, is plating under 90 ℃, and binding force of cladding material is good, but plating bath has a large amount of black nickels to separate out, and the plating bath of this moment is very unstable.
The preparation of plating bath: single nickel salt 25.0g/L, inferior sodium phosphate 8.0g/L, citric acid 70g/L, ammonium chloride 30.0g/L, sodium lauryl sulphate 0.003g/L.
The compound method of plating bath is identical with embodiment 1.
Embodiment 8
At first the simple clean surface of the most handy washing powder of silicon chip is washed with tap water, and distilled water flushing is put into the plating bath of stirring then, is plating under 60 ℃, and reaction is not carried out.
The preparation of plating bath: single nickel salt 25.0g/L, inferior sodium phosphate 8.0g/L, citric acid 70g/L, ammonium chloride 30.0g/L, sodium lauryl sulphate 0.005g/L.
The compound method of plating bath is: following all is to carry out at normal temperatures, and all churning time are all at 3～5 minutes
1. take by weighing single nickel salt, inferior sodium phosphate, citric acid, ammonium chloride, sodium lauryl sulphate by above-mentioned prescription and use the deionized water stirring and dissolving respectively, all every kind of amount of substances that every liter of deionized water need be put in the prescription, and will be by the good citric acid of deionized water dissolving, ammonium chloride, sodium lauryl sulphate remix;
2. with consoluet nickel salt solution, under constantly stirring, pour into and contain in the solution that 1. complex compound go on foot;
3. incite somebody to action consoluet sodium hypophosphite solution, under agitation, pour into by in the solution 2.;
4. with the good pH value conditioning agent of oneself dissolving, the pH value conditioning agent adopts the sulfuric acid of 5%NaOH solution or 10%, adds while stirring in the solution by 3. configuration, and surveying the pH value simultaneously is 8.0.
Embodiment 9
At first the simple clean surface of the most handy washing powder of silicon chip is washed with tap water, and distilled water flushing is put into the plating bath of stirring then, is plating under 60 ℃, and it is unstable that plating bath becomes, and have nickel to separate out, and binding force of cladding material is relatively poor.
The preparation of plating bath: single nickel salt 25.0g/L, inferior sodium phosphate 8.0g/L, citric acid 70g/L, ammonium chloride 20.0g/L, sodium lauryl sulphate 0.005g/L.
The compound method of plating bath is identical with embodiment 8, and recording the pH value is 10.0.
Claims (3)
1. alkali electroless plating bath is characterized in that: the weight part of forming electroplate liquid formulation is:
Main salt: single nickel salt 25.0～30.0
Buffer reagent: ammonium chloride 20～40
Complexing agent: citric acid 50～80
Reductive agent: inferior sodium phosphate 8.0～12.0
Stablizer: sodium lauryl sulphate 0.003～0.005.
2. the compound method of claim 1 alkali electroless plating bath is characterized in that:
A, single nickel salt, inferior sodium phosphate, citric acid, ammonium chloride, sodium lauryl sulphate are used the deionized water stirring and dissolving respectively, again citric acid, ammonium chloride, sodium lauryl sulphate are mixed;
B, with consoluet nickel salt solution, under constantly stirring, pour into and contain in the complex compound a mixing solutions in step;
C, general be consoluet sodium hypophosphite solution, under agitation, pours into by in the b solution in step;
D, the pH value conditioning agent that oneself dissolving is got well add while stirring by in the c solution in step, promptly obtain plating bath.
3. the plating bath method of claim 1 alkali electroless plating bath on silicon chip, it is characterized in that: silicon chip is immersed in the plating bath fully, is plating under 60 ℃.
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| CN 201110139693 CN102212804A (en) | 2011-05-27 | 2011-05-27 | Alkali chemical plating solution and solution plating method thereof on silicon chip |
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| CN 201110139693 CN102212804A (en) | 2011-05-27 | 2011-05-27 | Alkali chemical plating solution and solution plating method thereof on silicon chip |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105316663A (en) * | 2015-11-25 | 2016-02-10 | 江阴江化微电子材料股份有限公司 | Nickel-plating solution for preparing semiconductor silicon wafers |
-
2011
- 2011-05-27 CN CN 201110139693 patent/CN102212804A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| 《广州化工》 20110331 刘俊峰，胡弃疾，彭良富 环氧树脂板化学镀镍工艺研究 94-96 1－3 第39卷, 第5期 * |
| 《硕士研究生学位论文》 20071231 万家瑰 铝质基材表面纳米复合镀层实验研究 17－18 2－3 , * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105316663A (en) * | 2015-11-25 | 2016-02-10 | 江阴江化微电子材料股份有限公司 | Nickel-plating solution for preparing semiconductor silicon wafers |
| CN105316663B (en) * | 2015-11-25 | 2018-02-02 | 江阴江化微电子材料股份有限公司 | One kind prepares semi-conductor silicon chip nickel-plating liquid |
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Application publication date: 20111012 |