CN102010136A - Chemical plating Ni-P alloy technology of glass micro beads - Google Patents
Chemical plating Ni-P alloy technology of glass micro beads Download PDFInfo
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Abstract
The invention discloses a chemical plating Ni-P alloy technology of glass micro beads. A common chemical plating nickel liquid formula is adopted, the temperature is controlled to be 50-60 DEG C in the chemical plating nickel process, the plating application time is 30 minutes, and finally the chemical plated Ni-P alloy of glass micro bead with an even Ni-P deposition layer is obtained. After chemical plating, the contents of surface elements O and Si of the micro beads are lowered, but the contents of Ni and P are maximum, wherein the content of Ni reaches 58.76-68.41wt%, and the content of P reaches 8.87-10.04wt%. Compared with the chemical plating Ni-P alloy technology in the prior art, the content of Ni on the surface of the micro beads of the technology optimized by the invention is improved by 21.68-31.33wt%, and the content of P is improved by 8-9wt% compared with those of the technology which is not optimized.
Description
Technical field
The invention belongs to the electroless plating field of material surface, relate more specifically to a kind of glass microballon chemical plating Ni-P alloy process.
Background technology
Glass microballon has many particular performances, Mohs' hardness between 1.54-1.50, the intensity height, abrasion low, shock-resistant, stable chemical performance, and the glass microballon roundness is good, and size is evenly, the specific surface area height, cost is low, and good heat-resistant and good freedom from cracking performance are arranged.One of its application is the conductive filler material that can be used as behind the bead surface chemical Ni-P plating settled layer when electroplating, and reduces bath voltage, improves the quality of being plated part coating; Also can be used as the filler of electromagnetic shielding material and suction ripple stealth material.But for these application, the homogeneity of glass microballon surface metal coating is very important.
Present existing glass microballon chemical plating Ni-P alloy process, the bath temperature height, sedimentation velocity is fast, during the microballon electroless plating, easily form a large amount of free metal particles in the plating bath, cause the crystallization of bead surface Ni-P settled layer coarse, discontinuous, therefore bearing results is Ni-P settled layer lack of homogeneity.Simultaneously the content of Ni, the P of bead surface is owing to the reason of processing condition and operating method is lower, according to [10] bibliographical information, in the prior art after the glass microballon electroless plating content of Ni be 37.08% (wt), the content of P reaches 0.64% (wt).And the height of Ni, P content directly has influence on the crystal structure of Ni-P settled layer and the Corrosion Protection of settled layer in the glass microballon surface Ni-P settled layer.
Reference
[1] V.V.Budow and L.S.Egorova. Glass Microbeads, Application, Properties, and Technology (Review)[J]. Science in Glass Industry, 1994: 275-279
[2] Jiang Chunhua. the application of glass microballon [J]. Jiangsu building materials .2001,4:27-29
[3] Wang Guijun, Fan Hongbin, Song Liujiu, Xie Jun. the application [J] of glass microballon in matrix material. fibre composite, 2001,3:11-12
[4] Liu Baiyuan. the research [J] of superfine glass microballon (being called for short the microballon material). plastic working, 2003,38 (2):
36-41
[5] Zhang Zhen China, Meng Jinhong, Cao Xiaohui. hollow glass micropearl surface metalation and electromagnetic performance [J]. sufacing, 2006,35 (5): 10-11
[6] Ling Guoping. influence the inhomogeneity factor of hollow glass micropearl chemical nickel plating [J]. sufacing, 2004,33 (4): 19-21
[7] Chen Buming, Guo Zhongcheng, Yang Xianwan. tensio-active agent is to the research [J] of hollow glass micropearl chemical silvering influence. electroplate and finish 2007,26 (2): 25-28
[8] Chang Shiying, Guo Zhongcheng. Electroless silver plating on glass microbead [J]. electroplate and finish 2006,25 (11): 17-19
[9] Zheng Heng, Shao Qian, cold tree is big, Ge Shengsong. hollow glass micropearl surface no-palladium activating chemical nickel plating [J]. sufacing, 2008,37 (1): 56-58
[10] Yang Yuxiang, Shao Qian, Zheng Heng, Ge Shengsong. hollow glass micropearl chemical plating nickel-phosphorus alloy on surface [J].
Sufacing, 2007,36 (1): 39-42
[11] Mao Qianjin, in rosy clouds, Wang Qun etc. cenosphere surface metalation and electromagnetic protection performance study [J] thereof.
Beijing University of Technology's journal, 2003,29 (1): 108-111
[12] it is good etc. that Zhao Wen, Zhang Qiuyu, king tie. hollow glass micro-ball Study on Electroless Nickel [J]. and fine chemistry industry,
2005, 22(1):5-8。
Summary of the invention
The present invention is in order to solve problems such as above-mentioned Ni-P settled layer lack of homogeneity, glass microballon surface NI, P content are low, by optimizing bath temperature and plating time, adopt common chemical nickel plating liquid formula, analysis and composition test by glass microballon SEM before and after the plating and EDS can draw the uniform glass microballon chemical plating Mi-P alloy of Ni-P settled layer.
Technical scheme of the present invention
A kind of glass microballon chemical plating Ni-P alloy process comprises the steps:
(1), the oil removing of glass microballon ultrasonic wave, the ultrasonic wave degreasing fluid form and the content proportioning as follows:
Sodium hydroxide 5～10g/L
Sodium phosphate 30～35 g/L
OP-10 emulsifying agent 5～10 mL/L
The ultrasonic procedure controlled temperature is 20～30 ℃, and time 3min topples over then and electrolytic solution, and cleaning glass microballon with distilled water has oil removing electrolytic solution until bead surface is not residual;
(2),The glass microballon sensitization, the proportioning of sensitization electrolytic solution composition and content thereof is as follows:
Hydrochloric acid (37%) 50 ~ 100 mL/L
The glass microballon of step (1) after the ultrasonic wave oil removing inserted sensitization in the sensitization electrolytic solution, the sensitizing controlled temperature is 20～30 ℃, sensitization time is 2min, topples over then sensitization electrolytic solution, and cleaning glass microballon with distilled water has sensitization electrolytic solution until bead surface is not residual;
(3),The glass microballon activation, activated electrolyte composition and content proportioning are as follows:
Palladous chloride 0.5 ~ 1g/L
Hydrochloric acid (37%) 10 ~ 15 mL/L
To insert in the activated electrolyte through the glass microballon after step (2) sensitization is handled and activate, reactivation process control pH is 1.5 ~ 2.5, and temperature is 20 ~ 30 ℃, and soak time is 3min, topple over then and electrolytic solution, cleaning glass microballon with distilled water has an activated electrolyte until bead surface is not residual;
(4),The glass microballon chemical Ni-P plating, the proportioning of chemical nickel phosphorus plating electrolytic solution composition and content is as follows:
Single nickel salt 25 ~ 30 g/L
Inferior sodium phosphate 25 ~ 30 g/L
Sodium-acetate 10 ~ 20 g/L
Glass microballon after the activated processing in the step (3) inserted carry out electroless plating in the chemical nickel phosphorus plating electrolytic solution, control pH is 4.5～5.5 in the chemical Ni-P plating process, temperature is 50～60 ℃, plating time is 30min, the back is cleaned 3-4 time and is placed the loft drier controlled temperature to be 25 ℃ with distilled water and dries, finally obtain the uniform glass microballon chemical plating Mi-P alloy of Ni-P settled layer.
In the above-mentioned glass microballon chemical Ni-P plating technology, the cleaning between the microballon pretreatment procedure is very important.Microballon small-sized flows easily, and not contaminated for the quality and the electrolytic solution that guarantee coating, the cleaning of inter process under agitation could be cleaned more than at least 3 times.
In addition, select the plating temperature of chemical Ni-P plating electrolytic solution also very crucial; When being heated to 85～90 ℃ glass microballon is carried out electroless plating as if temperature with chemical Ni-P plating electrolytic solution, because electroless plating reaction speed was very fast when temperature was high, the metal Ni that separates out in a large number has little time to cover the glass microballon surface, so that be scattered in the plating bath and between microballon more metallic particles is arranged, cause the uneven coating of microparticle surfaces even, discontinuous, coating blackout, most of bead surface even do not have coating.If bath temperature is too high in addition, also can cause the decomposition of inferior sodium phosphate, cause the rising of plating bath foreign matter content, plating bath to lose efficacy.
Beneficial effect of the present invention
The present invention adopts common chemical nickel plating liquid formula, by optimize bath temperature and time when changing to the inhomogeneity influence of bead surface chemical Ni-P plating settled layer, analysis and composition test by glass microballon SEM before and after the plating and EDS finally obtain the uniform glass microballon chemical plating Mi-P alloy of Ni-P settled layer.And descend through bead surface element O, Si content after the electroless plating, and Ni, P content are maximum, and wherein the content of Ni reaches 58.76～68.41% (wt), and the content of P reaches 8.87% (wt)-10.04% (wt).According to document [10], in the prior art after the glass microballon electroless plating content of Ni reach 37.08% (wt), the content of P reaches 0.64% (wt), therefore Ni in the settled layer that obtains, P content is on the low side, the settled layer crystal structure is not a non-crystalline state, and the Corrosion Protection of settled layer is poor.And the raising that the content of the bead surface Ni of the technology of the present invention after optimizing is not more optimized 21.68～31.33% (wt), the raising that the content of P is not more optimized 8% (wt)-9% (wt), the Ni-P settled layer is the non-crystalline state crystal structure, and the Corrosion Protection of settled layer is better.
Description of drawings
85 ℃ of Fig. 1 a, bath temperatures, the SEM pattern of microballon during plating time 30min (amplifying 60 times)
85 ℃ of Fig. 1 b, bath temperatures, the SEM pattern of bead surface coating during plating time 30min (amplifying 2000 times)
60 ℃ of Fig. 2 a, bath temperatures, the SEM pattern of microballon during plating time 30min (amplifying 55 times)
60 ℃ of Fig. 2 b, bath temperatures, the SEM pattern of bead surface coating during plating time 30min (amplifying 2000 times)
The EDS figure of Fig. 3, electroless plating front glass bead surface
60 ℃ of Fig. 4, bath temperatures, the EDS on settled layer surface figure after the glass microballon electroless plating
50 ℃ of Fig. 5 a, bath temperatures, the SEM pattern of microballon during plating time 30min (amplifying 60 times)
50 ℃ of Fig. 5 b, bath temperatures, the SEM pattern of bead surface coating during plating time 30min (amplifying 2000 times)
50 ℃ of Fig. 6, bath temperatures, the EDS on settled layer surface figure after the glass microballon electroless plating.
Embodiment
Below by embodiment the present invention is further set forth, but do not limit the present invention.
The raw material that the present invention is used: diameter is the solid glass micro-bead of 0.6～0.8mm.
The reagent that the present invention is used: single nickel salt, inferior sodium phosphate, Trisodium Citrate, sodium-acetate, sodium hydroxide,
Tertiary sodium phosphate, yellow soda ash, tin protochloride, hydrochloric acid, Palladous chloride etc., above reagent is commercially available analytical reagent.
The OP-10 emulsifying agent that the present invention is used: analytical pure, Wuxi City spirit reach chemical reagent factory and produce.
The testing tool that the present invention is used: the 3400N scanning electron microscope of FDAC, the QUANTAX energy depressive spectroscopy of German Bruker
Embodiment 1
A kind of glass microballon chemical plating Ni-P alloy process comprises the steps:
(1), the oil removing of glass microballon ultrasonic wave, the ultrasonic wave degreasing fluid form and the content proportioning as follows:
Sodium hydroxide 10 g/L
Yellow soda ash 15g/L
Sodium phosphate 35 g/L
OP-10 emulsifying agent 10 mL/L
The ultrasonic procedure controlled temperature is 25 ℃, and time 3min topples over then and electrolytic solution, cleans glass microballon 4 times with distilled water, oil removing electrolytic solution is arranged until bead surface is not residual;
(2), the glass microballon sensitization, sensitizing solution form and the proportioning of content as follows:
Tin protochloride 15 g/L
Hydrochloric acid (content 37%) 100 mL/L
The sensitizing controlled temperature is 25 ℃, and sensitization time is 2min, topples over then electrolytic solution, cleans glass microballon 4 times with distilled water, sensitization electrolytic solution is arranged until bead surface is not residual;
(3), glass microballon activation, activation solution form and the content proportioning as follows
Palladous chloride 1g/L
Hydrochloric acid (content 37%) 15 mL/L
Reactivation process control pH is 2.5, and temperature is 25 ℃, and soak time is 3min, topples over then electrolytic solution, cleans glass microballon 4 times with distilled water, activated electrolyte is arranged until bead surface is not residual;
(4), the glass microballon chemical Ni-P plating, chemical nickel-plating liquid form and the proportioning of content as follows:
Single nickel salt 30 g/L
Inferior sodium phosphate 30 g/L
Sodium-acetate 20 g/L
Trisodium Citrate 20 g/L
Control pH is 5.0 in the chemical Ni-P plating process, temperature is 85 ℃, after glass microballon put into plating bath, stir plating bath and make it to be uniformly dispersed, and stir in plating process discontinuous, intermittent time 5min, churning time 5min, plating time is 30min, plating is finished hypsokinesis and is poured out chemical plating fluid, clean behind the glass microballon 4 times and place the loft drier controlled temperature to be 25 ℃ with distilled water and dry, finally form Ni-P alloy deposition layer in bead surface
Above-mentioned in the process of carrying out the glass microballon chemical plating Mi-P alloy 85 ℃ of bath temperatures, the SEM pattern of microballon during plating time 30min (amplifying 60 times) is seen Fig. 1 a, 85 ℃ of bath temperatures, the SEM pattern of bead surface coating during plating time 30min (amplifying 2000 times) is seen Fig. 1 b.
By Fig. 1 a and Fig. 1 b as can be seen, glass microballon is through after the electroless plating, and the bead surface major part has coated one deck settled layer, but settled layer is inhomogeneous, and the settled layer crystal structure presents dendritic structure.In conjunction with observed phenomenon in the experiment, illustrate that when bath temperature is high the glass microballon surface can not obtain satisfied Ni-P settled layer.
A kind of glass microballon chemical plating Ni-P alloy process comprises the steps:
(1), with embodiment 1;
(2), with embodiment 1;
(3), with embodiment 1;
(4), 60 ℃ of controlled temperature in the chemical Ni-P plating process, other conditions are with embodiment 1.
Glass microballon is put into the plating bath discontinuous to be stirred when carrying out electroless plating, because electroless plating reaction speed is moderate under this temperature, therefore, all bead surface can form evenly, continuously, the Ni-P alloy deposition layer of light, there is not the free metallic particles to exist in the plating bath and between microballon, Fig. 2 a and Fig. 2 b are 60 ℃ of bath temperatures, the SEM pattern of microballon and bead surface coating during plating time 30min, draw by Fig. 2 a and Fig. 2 b, glass microballon is when bath temperature is low after the electroless plating, it is even that bead surface has coated one deck, continuously, the settled layer of light, the settled layer densification.
Fig. 3 and Fig. 4 are respectively embodiment 2, and controlled temperature is the glass microballon EDS spectrogram after 60 ℃ the plating before the glass microballon plating and in the chemical Ni-P plating process.Can draw electroless plating front glass bead surface element based on O, Ca, Si, Na from Fig. 3 and Fig. 4, the content of other element seldom.Descend through bead surface element O, Si content after the electroless plating, and Ni, P content (Ni content is that 61.41% (wt), P content are 8.87% (wt)) at most, this settled layer that has just confirmed the microballon plating rear surface seen in the scanning electron microscope is the Ni-P alloy.Also observe other element on the EDS after the glass microballon electroless plating can spectrogram, this is because the chemical Ni-P plating settled layer is thinner, and electron beam is injected the thin place of coating, makes the element that has occurred the trace that microballon itself contained in the spectrogram.
Embodiment 3
A kind of glass microballon chemical plating Ni-P alloy process comprises the steps:
(1), the oil removing of glass microballon ultrasonic wave, the ultrasonic wave degreasing fluid form and the content proportioning as follows:
Sodium hydroxide 5 g/L
Yellow soda ash 10g/L
Sodium phosphate 30 g/L
OP-10 emulsifying agent 5 mL/L
The ultrasonic procedure controlled temperature is 25 ℃, and time 3min topples over then and electrolytic solution, cleans glass microballon 4 times with distilled water, oil removing electrolytic solution is arranged until bead surface is not residual;
(2), the glass microballon sensitization, sensitizing solution form and the proportioning of content as follows:
Tin protochloride 10 g/L
Hydrochloric acid (content 37%) 50 mL/L
The sensitizing controlled temperature is 25 ℃, and sensitization time is 2min, topples over then electrolytic solution, cleans glass microballon 4 times with distilled water, sensitization electrolytic solution is arranged until bead surface is not residual;
(3), glass microballon activation, activation solution form and the content proportioning as follows
Palladous chloride 0.5g/L
Hydrochloric acid (content 37%) 10 mL/L
Reactivation process control pH is 2.0, and temperature is 25 ℃, and soak time is 3min, topples over then electrolytic solution, cleans glass microballon 4 times with distilled water, activated electrolyte is arranged until bead surface is not residual;
(4), the glass microballon chemical Ni-P plating, chemical nickel-plating liquid form and the proportioning of content as follows:
Single nickel salt 25 g/L
Inferior sodium phosphate 25 g/L
Sodium-acetate 10 g/L
Trisodium Citrate 10 g/L
Control pH is 5.0 in the chemical Ni-P plating process, temperature is 50 ℃, after glass microballon put into plating bath, stir plating bath and make it to be uniformly dispersed, and stir in plating process discontinuous, intermittent time 10min, churning time 5min, plating time is 30min, plating is finished hypsokinesis and is poured out chemical plating fluid, clean behind the glass microballon 4 times and place the loft drier controlled temperature to be 25 ℃ with distilled water and dry, finally form even, continuous, bright Ni-P alloy deposition layer in bead surface
Fig. 5 a and Fig. 5 b are 50 ℃ of bath temperatures, the SEM pattern of microballon and bead surface coating during plating time 30min is drawn by Fig. 5 a and Fig. 5 b, and glass microballon is when bath temperature is low after the electroless plating, bead surface coated one deck evenly, the successive settled layer, the settled layer densification.
Fig. 6 is embodiment 3, the glass microballon EDS spectrogram when controlled temperature is 50 ℃ in the glass microballon chemical Ni-P plating process after the plating.From Fig. 6, can draw through bead surface element O, Si content after the electroless plating and descend, and Ni, P content (Ni content is that 58.76% (wt), P content are 10.04% (wt)) at most, the settled layer of glass microballon electroless plating rear surface is the Ni-P alloy.
A kind of glass microballon chemical plating Ni-P alloy process comprises the steps:
(1), the oil removing of glass microballon ultrasonic wave, the ultrasonic wave degreasing fluid form and the content proportioning as follows:
Sodium hydroxide 8.5g/L
Yellow soda ash 12g/L
Sodium phosphate 32 g/L
OP-10 emulsifying agent 7mL/L
The ultrasonic procedure controlled temperature is 25 ℃, and time 3min topples over then and electrolytic solution, cleans glass microballon 4 times with distilled water, oil removing electrolytic solution is arranged until bead surface is not residual;
(2), the glass microballon sensitization, sensitizing solution form and the proportioning of content as follows:
Tin protochloride 12 g/L
Hydrochloric acid (content 37%) 75 mL/L
The sensitizing controlled temperature is 25 ℃, and sensitization time is 2min, topples over then electrolytic solution, cleans glass microballon 4 times with distilled water, sensitization electrolytic solution is arranged until bead surface is not residual;
(3), glass microballon activation, activation solution form and the content proportioning as follows
Palladous chloride 0.8g/L
Hydrochloric acid (content 37%) 12 mL/L
Reactivation process control pH is 2.0, and temperature is 25 ℃, and soak time is 3min, topples over then electrolytic solution, cleans glass microballon 4 times with distilled water, activated electrolyte is arranged until bead surface is not residual;
(4), the glass microballon chemical Ni-P plating, chemical nickel-plating liquid form and the proportioning of content as follows:
Single nickel salt 28 g/L
Inferior sodium phosphate 30g/L
Sodium-acetate 15 g/L
Trisodium Citrate 15 g/L
Control pH is 5.0 in the chemical Ni-P plating process, temperature is 55 ℃, after glass microballon put into plating bath, stir plating bath and make it to be uniformly dispersed, and stir in plating process discontinuous, intermittent time 10min, churning time 5min, plating time is 30min, plating is finished hypsokinesis and is poured out chemical plating fluid, clean behind the glass microballon 4 times and place the loft drier controlled temperature to be 25 ℃ with distilled water and dry, finally form even, continuous, bright Ni-P alloy deposition layer in bead surface
In sum, solid glass micro-bead is through technology of the present invention, when the chemical plating fluid temperature is low, glass microballon does not have agglomeration in plating bath, can form even, continuous, fine and close Ni-P alloy deposition layer in bead surface, settled layer outward appearance light, the content of Ni is 58.76～68.41% (wt) in the Ni-P alloy deposition layer, the content of P is 8.87-10.04% (wt).
Under the prerequisite that does not depart from operational path of the present invention and essence, can carry out various modifications and change to the present invention, these modifications and change all belong within the scope of appended claims.
Claims (5)
1. a glass microballon chemical plating Ni-P alloy process is characterized in that controlled temperature is 50～60 ℃ in the electroless plating process, and plating time is 30min.
2. a kind of glass microballon chemical plating Ni-P alloy process as claimed in claim 1 is characterized in that comprising following concrete steps:
(1), the oil removing of glass microballon ultrasonic wave, the ultrasonic wave degreasing fluid form and the content proportioning as follows:
Sodium hydroxide 5～10g/L
Yellow soda ash 10～15g/L
Sodium phosphate 30～35g/L
OP-10 emulsifying agent 5～10mL/L
The ultrasonic procedure controlled temperature is 20～30 ℃, and time 3min topples over then and electrolytic solution, and cleaning glass microballon with distilled water has oil removing electrolytic solution until bead surface is not residual;
(2), the glass microballon sensitization, sensitization electrolytic solution form and the proportioning of content as follows:
Tin protochloride 10～15g/L
Hydrochloric acid (37%) 50～100mL/L
The glass microballon of step (1) after the ultrasonic wave oil removing inserted sensitization in the sensitization electrolytic solution, the sensitizing controlled temperature is 20～30 ℃, sensitization time is 2min, topples over then sensitization electrolytic solution, and cleaning glass microballon with distilled water has sensitization electrolytic solution until bead surface is not residual;
(3), glass microballon activation, activated electrolyte form and the content proportioning as follows:
Palladous chloride 0.5～1g/L
Hydrochloric acid (37%) 10～15mL/L
To insert in the activated electrolyte through the glass microballon after step (2) sensitization is handled and activate, reactivation process control pH is 1.5～2.5, and temperature is 20～30 ℃, and soak time is 3min, topple over then and electrolytic solution, cleaning glass microballon with distilled water has an activated electrolyte until bead surface is not residual;
(4), the glass microballon chemical Ni-P plating, chemical nickel phosphorus plating electrolytic solution form and the proportioning of content as follows:
Single nickel salt 25～30 g/L
Inferior sodium phosphate 25～30 g/L
Sodium-acetate 10～20 g/L
Trisodium Citrate 10～20 g/L
Glass microballon after the activated processing in the step (3) inserted carry out electroless plating in the chemical nickel phosphorus plating electrolytic solution, control pH is 4.5～5.5 in the chemical Ni-P plating process, temperature is 50～60 ℃, plating time is 30min, the back is cleaned 3-4 time and is placed the loft drier controlled temperature to be 25 ℃ with distilled water and dries, finally obtain the uniform glass microballon chemical plating Mi-P alloy of Ni-P settled layer.
3. a kind of glass microballon chemical plating Ni-P alloy process as claimed in claim 2 is characterized in that:
Glass microballon ultrasonic wave oil removing in the step (1), ultrasonic wave degreasing fluid composition and content proportioning are as follows:
Sodium hydroxide 10 g/L
Yellow soda ash 15 g/L
Sodium phosphate 35 g/L
OP-10 emulsifying agent 10 mL/L
The ultrasonic procedure controlled temperature is 25 ℃, and time 3min topples over then and electrolytic solution, and cleaning glass microballon with distilled water has oil removing electrolytic solution until bead surface is not residual;
Glass microballon sensitization in the step (2), the proportioning of sensitizing solution composition and content thereof is as follows:
Tin protochloride 15 g/L
Hydrochloric acid (content 37%) 100 mL/L
The sensitizing controlled temperature is 25 ℃, and sensitization time is 2min, topples over then electrolytic solution, cleans glass microballon 4 times with distilled water;
Glass microballon activation in the step (3), activation solution composition and content proportioning are as follows
Palladous chloride 1 g/L
Hydrochloric acid (content 37%) 15 mL/L
Reactivation process control pH is 2.5, and temperature is 25 ℃, and soak time is 3min, topples over then electrolytic solution, cleans glass microballon 4 times with distilled water;
Glass microballon chemical Ni-P plating in the step (4), the proportioning of chemical nickel-plating liquid composition and content is as follows:
Single nickel salt 30 g/L
Inferior sodium phosphate 30 g/L
Sodium-acetate 20 g/L
Trisodium Citrate 20 g/L
Control pH is 5.0 in the chemical Ni-P plating process, temperature is 60 ℃, after glass microballon put into plating bath, stir plating bath and make it to be uniformly dispersed, and stir in plating process discontinuous, intermittent time 5min, churning time 5min, plating time is 30min, plating is finished hypsokinesis and is poured out chemical plating fluid, clean behind the glass microballon 4 times and place the loft drier controlled temperature to be 25 ℃ with distilled water and dry, finally form Ni-P alloy deposition layer in bead surface
4. a kind of glass microballon chemical plating Ni-P alloy process as claimed in claim 2 is characterized in that:
Glass microballon ultrasonic wave oil removing in the step (1), ultrasonic wave degreasing fluid composition and content proportioning are as follows:
Sodium hydroxide 5 g/L
Yellow soda ash 10 g/L
Sodium phosphate 30 g/L
OP-10 emulsifying agent 5 mL/L
The ultrasonic procedure controlled temperature is 25 ℃, and time 3min topples over then and electrolytic solution, cleans glass microballon 4 times with distilled water, oil removing electrolytic solution is arranged until bead surface is not residual;
Glass microballon sensitization in the step (2), the proportioning of sensitizing solution composition and content thereof is as follows:
Tin protochloride 10 g/L
Hydrochloric acid (content 37%) 50 mL/L
The sensitizing controlled temperature is 25 ℃, and sensitization time is 2min, topples over then electrolytic solution, cleans glass microballon 4 times with distilled water, sensitization electrolytic solution is arranged until bead surface is not residual;
Glass microballon activation in the step (3), activation solution composition and content proportioning are as follows:
Palladous chloride 0.5g/L
Hydrochloric acid (content 37%) 10 mL/L
Reactivation process control pH is 2.0, and temperature is 25 ℃, and soak time is 3min, topples over then electrolytic solution, cleans glass microballon 4 times with distilled water, activated electrolyte is arranged until bead surface is not residual;
Glass microballon chemical Ni-P plating in the step (4), the proportioning of chemical nickel-plating liquid composition and content is as follows:
Single nickel salt 25 g/L
Inferior sodium phosphate 25 g/L
Sodium-acetate 10 g/L
Trisodium Citrate 10 g/L
Control pH is 5.0 in the chemical Ni-P plating process, temperature is 50 ℃, after glass microballon put into plating bath, stir plating bath and make it to be uniformly dispersed, and stir in plating process discontinuous, intermittent time 10min, churning time 5min, plating time is 30min, plating is finished hypsokinesis and is poured out chemical plating fluid, clean behind the glass microballon 4 times and place the loft drier controlled temperature to be 25 ℃ with distilled water and dry, finally form Ni-P alloy deposition layer in bead surface
5. a kind of glass microballon chemical plating Ni-P alloy process as claimed in claim 2 is characterized in that:
Glass microballon ultrasonic wave oil removing in the step (1), ultrasonic wave degreasing fluid composition and content proportioning are as follows:
Sodium hydroxide 8.5 g/L
Yellow soda ash 12 g/L
Sodium phosphate 32 g/L
OP-10 emulsifying agent 7mL/L
The ultrasonic procedure controlled temperature is 25 ℃, and time 3min topples over then and electrolytic solution, cleans glass microballon 4 times with distilled water, oil removing electrolytic solution is arranged until bead surface is not residual;
Glass microballon sensitization in the step (2), the proportioning of sensitizing solution composition and content thereof is as follows:
Tin protochloride 12 g/L
Hydrochloric acid (content 37%) 75 mL/L
The sensitizing controlled temperature is 25 ℃, and sensitization time is 2min, topples over then electrolytic solution, cleans glass microballon 4 times with distilled water, sensitization electrolytic solution is arranged until bead surface is not residual;
Glass microballon activation in the step (3), activation solution composition and content proportioning are as follows:
Palladous chloride 0.8 g/L
Hydrochloric acid (content 37%) 12 mL/L
Reactivation process control pH is 2.0, and temperature is 25 ℃, and soak time is 3min, topples over then electrolytic solution, cleans glass microballon 4 times with distilled water, activated electrolyte is arranged until bead surface is not residual;
Glass microballon chemical Ni-P plating in the step (4), the proportioning of chemical nickel-plating liquid composition and content is as follows:
Single nickel salt 28 g/L
Inferior sodium phosphate 30 g/L
Sodium-acetate 15 g/L
Trisodium Citrate 15 g/L
Control pH is 5.0 in the chemical Ni-P plating process, temperature is 55 ℃, after glass microballon put into plating bath, stir plating bath and make it to be uniformly dispersed, and stir in plating process discontinuous, intermittent time 10min, churning time 5min, plating time is 30min, plating is finished hypsokinesis and is poured out chemical plating fluid, clean behind the glass microballon 4 times and place the loft drier controlled temperature to be 25 ℃ with distilled water and dry, finally form Ni-P alloy deposition layer in bead surface
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| CN104018139A (en) * | 2014-06-20 | 2014-09-03 | 哈尔滨工业大学 | Hollow microsphere/Ni-Fe-P/Cu composite coating and preparation method thereof |
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| CN109183010B (en) * | 2018-11-01 | 2020-11-10 | 中钢集团马鞍山矿院新材料科技有限公司 | Method for roughening surface of hollow glass bead and plating nickel |
| CN110669324A (en) * | 2019-10-25 | 2020-01-10 | 中国建筑材料科学研究总院有限公司 | Conductive glass fiber reinforced plastic, conductive glass fiber reinforced plastic plate and preparation method thereof |
| CN110669324B (en) * | 2019-10-25 | 2022-05-27 | 中国建筑材料科学研究总院有限公司 | Conductive glass fiber reinforced plastic, conductive glass fiber reinforced plastic plate and preparation method thereof |
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