CN108893730B - Plating solution and method for chemically plating pearl nickel - Google Patents
Plating solution and method for chemically plating pearl nickel Download PDFInfo
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- CN108893730B CN108893730B CN201810775371.5A CN201810775371A CN108893730B CN 108893730 B CN108893730 B CN 108893730B CN 201810775371 A CN201810775371 A CN 201810775371A CN 108893730 B CN108893730 B CN 108893730B
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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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
- C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
- C23C18/36—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents using hypophosphites
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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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1803—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces
- C23C18/1824—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by chemical pretreatment
- C23C18/1837—Multistep pretreatment
- C23C18/1844—Multistep pretreatment with use of organic or inorganic compounds other than metals, first
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Abstract
A plating solution and a method for chemically plating pearl nickel relate to a pretreatment method on a low-carbon steel sheet and a preparation method by utilizing the plating solution for chemically plating the pearl nickel. The invention aims to solve the problems of complex instrument, accurate operation, difficult control, poor coating uniformity and the like in the traditional pearl nickel preparation method. The method of the invention comprises the following steps: firstly, preparing alkaline washing liquid; secondly, preparing surface pre-plating solution; thirdly, preparing chemical plating solution; fourthly, the preparation process flow of pearl nickel is as follows: acid cleaning and rust removing → mechanical polishing → water cleaning → alkali cleaning and oil removing → water cleaning → acid cleaning and activation → water cleaning → blow drying → preplating → chemical plating. The pearl nickel prepared by the invention has uniform plating layer, and can reduce consumption in the process aspect, thereby saving energy and reducing emission.
Description
Technical Field
The invention relates to a pearl nickel plating process and plating solution, in particular to plating solution and a method for chemically plating pearl nickel.
Background
Electroless nickel plating is a process for depositing a layer of nickel on the surface of a metallic article by redox without the use of an external current. Used for improving corrosion resistance and wear resistance, and increasing luster and beauty. It is suitable for bright nickel plating of tubular or complex-shaped small parts without polishing. Generally, a plated part is immersed in a mixed solution prepared from nickel sulfate, sodium hypophosphite, sodium acetate and boric acid, and changes under a certain acidity and temperature, so that nickel ions in the solution are reduced into atoms by the sodium hypophosphite and deposited on the surface of the part to form a fine and bright nickel plating layer.
Pearl nickel is also known as satin nickel, salbutamol nickel, etc. Because of the unique surface appearance, the pearl bright nickel alloy has pearly elegant luster on visual sense, does not reflect light strongly like bright nickel, and makes people feel comfortable. Therefore, the pearl nickel does not cause visual fatigue after being observed for a long time, so people can select more pearl nickel products at present, and the pearl nickel is favored in the fields of aerospace, life and scientific research. The pearl nickel has unsmooth and uneven surfaces, light can be subjected to diffuse reflection on the surfaces, meanwhile, the porosity is low, the internal stress is lower than that of normal bright nickel and dark nickel, the corrosion resistance is good, and fingerprints cannot be easily left by touching with hands. At present, pearl nickel is adopted and popularized as one of corrosion-resistant materials in many European and American countries, Japan and the like.
Disclosure of Invention
The invention aims to provide a plating solution and a method for preparing pearl nickel by chemical plating, which solve the problems of monotonous preparation method, uneven plating layer and the like of the pearl nickel.
The invention relates to a plating solution and a method for chemically plating pearl nickel, which are carried out according to the following steps:
firstly, preparing an alkaline washing solution: dissolving sodium hydroxide, sodium phosphate, sodium silicate, sodium carbonate and sodium dodecyl sulfate in deionized water for later use;
secondly, preparing a pre-plating solution: dissolving zinc oxide, zinc dihydrogen phosphate, phosphoric acid, citric acid, sodium fluoride, sodium dodecyl benzene sulfonate and sodium molybdate in deionized water, and adjusting the pH value for later use;
thirdly, preparing chemical plating solution:
(1) acid electroless plating solution: dissolving nickel sulfate, sodium hypophosphite, citric acid, anhydrous sodium acetate, sodium chloride, an emulsifier OP-10, potassium iodate and sodium dihexyl succinate sulfonate in deionized water, and adjusting the pH value for later use;
(2) alkaline electroless plating solution: dissolving nickel sulfate, sodium hypophosphite, sodium citrate, anhydrous sodium acetate, sodium chloride, an emulsifier OP-10, potassium iodate and sodium dihexyl succinate sulfonate in deionized water, and adjusting the pH value for later use;
fourthly, preparing a pickling solution in a pickling and rust removing process, then putting the low-carbon steel sheet into the pickling solution for pickling and rust removing, then performing mechanical polishing, taking out and washing, after washing, putting into an alkali washing solution for removing oil, after removing oil, taking out and washing, then performing pickling and activation, after activation, washing, drying, putting into a pre-plating solution for surface pre-plating, finally putting into a chemical plating solution for plating, after finishing, washing, and drying.
The invention has the following beneficial effects:
compared with the prior art, the pearl nickel has the advantages of good corrosion resistance, uniform plating layer, easier control and the like. The method for chemically plating the pearl nickel changes a single preparation method of the pearl nickel, has simpler operation, low cost and high utilization rate, can save resources and achieve the advantages of economy and environmental protection.
Drawings
FIG. 1 is an appearance diagram of a nickel-plated product, wherein a is bright nickel, b is semi-bright nickel, c is dark nickel, and d is pearl nickel.
FIG. 2 is a Scanning Electron Microscope (SEM) image (2000X) of pearl nickel.
FIG. 3 is a Scanning Electron Microscope (SEM) image (10000X) of pearl nickel.
Detailed Description
The present invention is further illustrated by the following examples, which should not be construed as limiting the scope of the invention.
The first embodiment is as follows: the plating solution and the method for chemically plating pearl nickel in the embodiment are carried out according to the following steps:
firstly, preparing an alkaline washing solution: dissolving sodium hydroxide, sodium phosphate, sodium silicate, sodium carbonate and sodium dodecyl sulfate in deionized water for later use;
secondly, preparing a pre-plating solution: dissolving zinc oxide, zinc dihydrogen phosphate, phosphoric acid, citric acid, sodium fluoride, sodium dodecyl benzene sulfonate and sodium molybdate in deionized water, and adjusting the pH value for later use;
thirdly, preparing chemical plating solution:
(1) acid electroless plating solution: dissolving nickel sulfate, sodium hypophosphite, citric acid, anhydrous sodium acetate, sodium chloride, an emulsifier OP-10, potassium iodate and sodium dihexyl succinate sulfonate in deionized water, and adjusting the pH value for later use;
(2) alkaline electroless plating solution: dissolving nickel sulfate, sodium hypophosphite, sodium citrate, anhydrous sodium acetate, sodium chloride, an emulsifier OP-10, potassium iodate and sodium dihexyl succinate sulfonate in deionized water, and adjusting the pH value for later use;
fourthly, preparing a pickling solution in a pickling and rust removing process, then putting the low-carbon steel sheet into the pickling solution for pickling and rust removing, then performing mechanical polishing, taking out and washing, after washing, putting into an alkali washing solution for removing oil, after removing oil, taking out and washing, then performing pickling and activation, after activation, washing, drying, putting into a pre-plating solution for surface pre-plating, finally putting into a chemical plating solution for plating, after finishing, washing, and drying.
The second embodiment is as follows: the present embodiment is different from the specific embodiment in that: the alkaline solution oil removal process comprises the step one, removing saponifiable oil through the mechanisms of saponification, emulsification and soaking and wetting of alkaline solution to achieve the purpose of oil removal, wherein the alkaline solution is prepared by sequentially adding 90g/L sodium hydroxide, 30g/L sodium phosphate, 20g/L sodium silicate, 20g/L sodium carbonate and 0.02g/L sodium dodecyl sulfate into deionized water for dissolution. The rest is the same as the first embodiment.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: the formula of the pre-plating solution and the surface pre-plating process in the step two are as follows: preparing 150mL solution of 12g/L zinc oxide, 10g/L zinc dihydrogen phosphate, 30mL/L phosphoric acid, 0.5g/L citric acid, 0.4g/L sodium fluoride, 0.3g/L sodium dodecyl benzene sulfonate and 1g/L sodium molybdate in a 250mL beaker; dropwise adding concentrated ammonia water into the solution, adjusting the pH value to 2.5, finally immersing the activated steel sheet into the treatment solution for reaction, taking out after 15min of reaction, washing the surface with deionized water, and drying for later use. The others are the same as in the first or second embodiment.
The fourth concrete implementation mode: the present embodiment is different from the first to third embodiments in that: the formula and the process of the acidic chemical plating solution in the third step are as follows: preparing 100mL of solution containing 40g/L of nickel sulfate, 50g/L of sodium hypophosphite, 20g/L of citric acid, 20g/L of anhydrous sodium acetate, 20g/L of sodium chloride, 102.4-4.8 mL/L of emulsifier OP-0.0005-0.001 g/L of potassium iodate and 3.0mL/L of dihexyl sodium sulfosuccinate; dropwise adding concentrated ammonia water into the solution to adjust the pH value to 4-4.5, heating the solution to 85-90 ℃, putting the steel sheet with the pre-plated surface into a plating solution, performing plating reaction for 1.5h, taking out, washing with deionized water, and drying. The rest is the same as one of the first to third embodiments.
The fifth concrete implementation mode: the present embodiment is different from the first to the fourth embodiments in that: the formula and the process of the alkaline chemical plating solution in the third step are as follows: preparing 100mL of solution containing 40g/L of nickel sulfate, 50g/L of sodium hypophosphite, 20g/L of sodium citrate, 20g/L of anhydrous sodium acetate, 20g/L of sodium chloride, 102.4-4.8 mL/L of emulsifier OP-0.0005-0.001 g/L of potassium iodate and 3.0mL/L of dihexyl sodium sulfosuccinate; dropwise adding concentrated ammonia water into the solution to adjust the pH value to 9-9.5, heating the solution to 40-60 ℃, putting the steel sheet with the pre-plated surface into a plating solution, performing plating reaction for 1.5h, taking out, washing with deionized water, and drying. The rest is the same as one of the first to fourth embodiments.
The sixth specific implementation mode: the present embodiment is different from the first to fifth embodiments in that: the pickling rust removal solution and the process in the low-carbon steel pretreatment process are as follows: the pickling solution is prepared from deionized water and concentrated hydrochloric acid according to the volume ratio of 1:1, the pickling time is 5-10min, and the temperature is room temperature. The rest is the same as one of the first to fifth embodiments.
The inventive content is not limited to the embodiments described above, wherein combinations of one or several of the embodiments can equally well fulfill the objects of the invention.
The advantageous effects of the present invention are demonstrated by the following examples.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
The plating solution and the method for chemically plating pearl nickel in the embodiment mode are carried out according to the following steps:
firstly, preparing an alkaline washing solution: dissolving sodium hydroxide, sodium phosphate, sodium silicate, sodium carbonate and sodium dodecyl sulfate in deionized water for later use;
secondly, preparing a pre-plating solution: dissolving zinc oxide, zinc dihydrogen phosphate, phosphoric acid, citric acid, sodium fluoride, sodium dodecyl benzene sulfonate and sodium molybdate in deionized water, and adjusting the pH value for later use;
thirdly, preparing chemical plating solution:
(1) acid electroless plating solution: dissolving nickel sulfate, sodium hypophosphite, citric acid, anhydrous sodium acetate, sodium chloride, an emulsifier OP-10, potassium iodate and sodium dihexyl succinate sulfonate in deionized water, and adjusting the pH value for later use;
(2) alkaline electroless plating solution: dissolving nickel sulfate, sodium hypophosphite, sodium citrate, anhydrous sodium acetate, sodium chloride, an emulsifier OP-10, potassium iodate and sodium dihexyl succinate sulfonate in deionized water, and adjusting the pH value for later use;
fourthly, preparing a pickling solution in a pickling and rust removing process, then putting the low-carbon steel sheet into the pickling solution for pickling and rust removing, then performing mechanical polishing, taking out and washing, after washing, putting into an alkali washing solution for removing oil, after removing oil, taking out and washing, then performing pickling and activation, after activation, washing, drying, putting into a pre-plating solution for surface pre-plating, finally putting into a chemical plating solution for plating, after finishing, washing, and drying.
The alkaline solution oil removal process in the embodiment removes saponifiable oil through the mechanisms of saponification, emulsification and wetting of alkaline solution to achieve the purpose of oil removal, and the alkaline solution is prepared by sequentially adding 90g/L sodium hydroxide, 30g/L sodium phosphate, 20g/L sodium silicate, 20g/L sodium carbonate and 0.02g/L sodium dodecyl sulfate into deionized water for dissolution.
The formula of the pre-plating solution and the surface pre-plating process in the embodiment are as follows: preparing 150mL solution of 12g/L zinc oxide, 10g/L zinc dihydrogen phosphate, 30mL/L phosphoric acid, 0.5g/L citric acid, 0.4g/L sodium fluoride, 0.3g/L sodium dodecyl benzene sulfonate and 1g/L sodium molybdate in a 250mL beaker; dropwise adding concentrated ammonia water into the solution, adjusting the pH value to 2.5, finally immersing the activated steel sheet into the treatment solution for reaction, taking out after 15min of reaction, washing the surface with deionized water, and drying for later use.
The formula and the process of the acidic chemical plating solution in the embodiment are as follows: preparing 100mL of solution containing 40g/L of nickel sulfate, 50g/L of sodium hypophosphite, 20g/L of citric acid, 20g/L of anhydrous sodium acetate, 20g/L of sodium chloride, 102.4-4.8 mL/L of emulsifier OP-0.0005-0.001 g/L of potassium iodate and 3.0mL/L of dihexyl sodium sulfosuccinate; dropwise adding concentrated ammonia water into the solution to adjust the pH value to 4-4.5, heating the solution to 85-90 ℃, putting the steel sheet with the pre-plated surface into a plating solution, performing plating reaction for 1.5h, taking out, washing with deionized water, and drying.
The formula and the process of the alkaline chemical plating solution in the embodiment are as follows: preparing 100mL of solution containing 40g/L of nickel sulfate, 50g/L of sodium hypophosphite, 20g/L of sodium citrate, 20g/L of anhydrous sodium acetate, 20g/L of sodium chloride, 102.4-4.8 mL/L of emulsifier OP-0.0005-0.001 g/L of potassium iodate and 3.0mL/L of dihexyl sodium sulfosuccinate; dropwise adding concentrated ammonia water into the solution to adjust the pH value to 9-9.5, heating the solution to 40-60 ℃, putting the steel sheet with the pre-plated surface into a plating solution, performing plating reaction for 1.5h, taking out, washing with deionized water, and drying.
The pickling rust removal solution and the pickling rust removal process in the pretreatment process of the low-carbon steel in the embodiment are as follows: the pickling solution is prepared from deionized water and concentrated hydrochloric acid according to the volume ratio of 1:1, the pickling time is 5-10min, and the temperature is room temperature.
The appearance and Scanning Electron Microscope (SEM) of the pearl nickel prepared in this example are shown in fig. 1, 2, and 3, and the pearl nickel treated by the optimal formula has a uniform and dense surface, a pearl-like texture, and a jade-like luster.
The preparation process adopted by the embodiment is simple to operate, simple in flow, energy-saving and environment-friendly, and changes the single preparation process of the pearl nickel.
The corrosion resistance detection result of the pearl nickel prepared by the embodiment is that the corrosion resistance detection of the pearl nickel is carried out by using 41 g/L copper sulfate solution, and the rust point does not appear in 3 hours on average.
Claims (4)
1. A method for chemically plating pearl nickel is characterized by comprising the following steps: the method comprises the following steps:
firstly, preparing an alkaline washing solution: dissolving sodium hydroxide, sodium phosphate, sodium silicate, sodium carbonate and sodium dodecyl sulfate in deionized water for later use;
secondly, preparing a pre-plating solution: dissolving zinc oxide, zinc dihydrogen phosphate, phosphoric acid, citric acid, sodium fluoride, sodium dodecyl benzene sulfonate and sodium molybdate in deionized water, and adjusting the pH value for later use;
preparing chemical plating solution, wherein the chemical plating solution is acidic chemical plating solution or alkaline chemical plating solution
(1) Acid electroless plating solution: dissolving nickel sulfate, sodium hypophosphite, citric acid, anhydrous sodium acetate, sodium chloride, an emulsifier OP-10, potassium iodate and sodium dihexyl succinate sulfonate in deionized water, and adjusting the pH value for later use;
(2) alkaline electroless plating solution: dissolving nickel sulfate, sodium hypophosphite, sodium citrate, anhydrous sodium acetate, sodium chloride, an emulsifier OP-10, potassium iodate and sodium dihexyl succinate sulfonate in deionized water, and adjusting the pH value for later use;
fourthly, firstly preparing a pickling solution in a pickling and rust removing process, then putting the low-carbon steel sheet into the pickling solution for pickling and rust removing, then performing mechanical polishing, taking out and washing, after washing, putting into an alkali washing solution for oil removal, after oil removal, taking out and washing, then performing pickling and activation, after activation, washing, drying, putting into a pre-plating solution for surface pre-plating, finally putting into a chemical plating solution for plating, after completion, washing and drying;
the preparation process of the acidic electroless plating solution comprises the following steps: preparing 100mL of solution containing 40g/L of nickel sulfate, 50g/L of sodium hypophosphite, 20g/L of citric acid, 20g/L of anhydrous sodium acetate, 20g/L of sodium chloride, 102.4-4.8 mL/L of emulsifier OP-0.0005-0.001 g/L of potassium iodate and 3.0mL/L of dihexyl sodium sulfosuccinate; dropwise adding concentrated ammonia water into the solution to adjust the pH value to 4-4.5, heating the solution to 85-90 ℃, putting the steel sheet with the pre-plated surface into a plating solution, performing plating reaction for 1.5h, taking out, washing with deionized water, and drying;
the preparation process of the alkaline chemical plating solution comprises the following steps: preparing 100mL of solution containing 40g/L of nickel sulfate, 50g/L of sodium hypophosphite, 20g/L of sodium citrate, 20g/L of anhydrous sodium acetate, 20g/L of sodium chloride, 102.4-4.8 mL/L of emulsifier OP-0.0005-0.001 g/L of potassium iodate and 3.0mL/L of dihexyl sodium sulfosuccinate; dropwise adding concentrated ammonia water into the solution to adjust the pH value to 9-9.5, heating the solution to 40-60 ℃, putting the steel sheet with the pre-plated surface into a plating solution, performing plating reaction for 1.5h, taking out, washing with deionized water, and drying.
2. The method of claim 1, wherein: the alkali wash oil removal process is to remove saponifiable oil through the mechanisms of saponification, emulsification and soaking and wetting of alkali liquor to achieve the purpose of oil removal, and the formula of the alkali wash is that 90g/L of sodium hydroxide, 30g/L of sodium phosphate, 20g/L of sodium silicate, 20g/L of sodium carbonate and 0.02g/L of sodium dodecyl sulfate are sequentially added into deionized water to be dissolved.
3. The method of claim 1, wherein: the preparation and surface pre-plating process of the pre-plating solution comprises the following steps: preparing 150mL solution of 12g/L zinc oxide, 10g/L zinc dihydrogen phosphate, 30mL/L phosphoric acid, 0.5g/L citric acid, 0.4g/L sodium fluoride, 0.3g/L sodium dodecyl benzene sulfonate and 1g/L sodium molybdate in a 250mL beaker; dropwise adding concentrated ammonia water into the solution, adjusting the pH value to 2.5, finally immersing the activated steel sheet into the treatment solution for reaction, taking out after 15min of reaction, washing the surface with deionized water after taking out, and drying for later use.
4. The method of claim 1, wherein: the pickling solution and the process in the low-carbon steel sheet pickling and derusting process are as follows: the pickling solution is prepared from deionized water and concentrated hydrochloric acid according to the volume ratio of 1:1, the pickling time is 5-10min, and the temperature is room temperature.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101583330B1 (en) * | 2014-12-22 | 2016-01-07 | 대륙금속(주) | Satin-nickel plating method using the glossiness of the inspection |
| JP2017172017A (en) * | 2016-03-25 | 2017-09-28 | 株式会社Ｊｃｕ | Satin nickel plating bath and satin nickel plating method |
| WO2018066398A1 (en) * | 2016-10-07 | 2018-04-12 | 上村工業株式会社 | Nickel plating solution and nickel plating solution production method |
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2018
- 2018-07-16 CN CN201810775371.5A patent/CN108893730B/en active Active
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| KR101583330B1 (en) * | 2014-12-22 | 2016-01-07 | 대륙금속(주) | Satin-nickel plating method using the glossiness of the inspection |
| JP2017172017A (en) * | 2016-03-25 | 2017-09-28 | 株式会社Ｊｃｕ | Satin nickel plating bath and satin nickel plating method |
| WO2018066398A1 (en) * | 2016-10-07 | 2018-04-12 | 上村工業株式会社 | Nickel plating solution and nickel plating solution production method |
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| Title |
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| Remedies for common problems in pearl (satin) nickel electroplating;Zhu Zhuo-min，et al.;《Electroplating & Finishing》;20160615;第35卷(第11期);第579-581页 * |
| 珍珠镍电镀新工艺及其阴极过程初探;曹香雄;《中国优秀硕士学位论文全文数据库 工程科技I辑》;20161115(第11期);绪论 * |
| 装饰性沙丁镍镀层耐腐蚀性研究;陆纹雅;《中国优秀硕士学位论文全文数据库 工程科技I辑》;20130715(第7期);绪论 * |
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