CN102010136B - 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 chemical plating Ni-P alloy technology of glass micro beads.
Background technology
Glass microballon has the performance of many uniquenesses, and Mohs' hardness is between 1.54-1.50, and intensity is high, it is low, shock-resistant to wear away, stable chemical performance, and the glass microballon roundness is good, and size is evenly, specific surface area is high, and cost is low, and good resistance toheat and good freedom from cracking performance are arranged.One of its application is the conductive filler material can be used as after bead surface chemical Ni-P plating settled layer while electroplating, and reduces bath voltage, improves by the quality of plating 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.
Current existing chemical plating Ni-P alloy technology of glass micro beads, bath temperature is high, and sedimentation velocity is fast, during the microballon electroless plating, easily form a large amount of free metal particles in plating solution, 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 because the reason of processing condition and operating method is lower, according to [10] bibliographical information, in prior art after the glass microballon electroless plating content of Ni be 37.08% (wt), the content of P reaches 0.64% (wt).And in glass microballon surface Ni-P settled layer, 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.
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. affect the inhomogeneity factor of hollow glass micropearl chemical nickel plating [J]. sufacing, 2004,33 (4): 19-21
[7] Chen Buming, Guo Zhongcheng, Yang Xianwan. the research of influence of electroless silver plating on hollow glass microsphere by using surfactants [J]. 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. Palladium-free Activation Electroless Nickel Plating on Cenosphere Surface [J]. sufacing, 2008,37 (1): 56-58
[10] Yang Yuxiang, Shao Qian, Zheng Heng, Ge Shengsong. Electroless Ni-P Plating on Cenosphere 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] Zhao Wen, Zhang Qiuyu, it is good etc. that the king ties. Electroless Nickel Plating on Hollow Glass Microspheres research [J]. fine chemistry industry,
2005, 22(1):5-8。
Summary of the invention
The present invention is in order to solve the 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 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 chemical plating Ni-P alloy technology of glass micro beads, comprise 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
It is 20～30 ℃ that ultrasonic procedure is controlled temperature, and time 3min, then pour out electrolytic solution, and cleaning glass microballon with distilled water does not have oil removing electrolytic solution until bead surface is 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 to sensitization in sensitization electrolytic solution, it is 20～30 ℃ that sensitizing is controlled temperature, sensitization time is 2min, then pours out sensitization electrolytic solution, and cleaning glass microballon with distilled water does not have sensitization electrolytic solution until bead surface is 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
Glass microballon after step (2) sensitization is processed is inserted in activated electrolyte and activated, it is 1.5 ~ 2.5 that reactivation process is controlled pH, and temperature is 20 ~ 30 ℃, and soak time is 3min, then pour out electrolytic solution, cleaning glass microballon with distilled water does not have an activated electrolyte until bead surface is 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 activated processing in step (3) is inserted in chemical nickel phosphorus plating electrolytic solution and carried out electroless plating, controlling pH in the chemical Ni-P plating process is 4.5～5.5, temperature is 50～60 ℃, plating time is 30min, clean 3-4 time and be placed in loft drier control temperature with distilled water and be 25 ℃ and dried afterwards, finally obtain the uniform glass microballon chemical plating Mi-P alloy of Ni-P settled layer.
In above-mentioned glass microballon chemical Ni-P plating technique, the cleaning between the microballon pretreatment procedure is very important.Microballon small-sized, easily flow, 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; If when the temperature of chemical Ni-P plating electrolytic solution is heated to 85～90 ℃, glass microballon is carried out to electroless plating, due to temperature when high electroless plating reaction speed very fast, the metal Ni separated out in a large number has little time to cover the glass microballon surface, so that be scattered more metallic particles is arranged in plating solution and between microballon, cause the uneven coating of microparticle surfaces even, discontinuous, coating blackout, most of bead surface is even without coating.If bath temperature is too high in addition, also can cause the decomposition of inferior sodium phosphate, cause the rising of plating solution foreign matter content, plating solution 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 while changing on the inhomogeneity impact of bead surface chemical Ni-P plating settled layer, analysis and composition test by glass microballon SEM before and after plating and EDS, finally obtain the uniform glass microballon chemical plating Mi-P alloy of Ni-P settled layer.And bead surface element O, Si content descend after 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 prior art after the glass microballon electroless plating content of Ni reach 37.08% (wt), the content of P reaches 0.64% (wt), Ni in the settled layer therefore obtained, P content is on the low side, the settled layer crystal structure is not 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 technique 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.
The accompanying drawing explanation
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: the solid glass micro-bead that diameter is 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, sodium carbonate, 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, the Wuxi City spirit reaches chemical reagent factory and produces.
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 chemical plating Ni-P alloy technology of glass micro beads, comprise 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
Sodium carbonate 15g/L
Sodium phosphate 35 g/L
OP-10 emulsifying agent 10 mL/L
It is 25 ℃ that ultrasonic procedure is controlled temperature, and time 3min, then pour out electrolytic solution, with distilled water, cleans glass microballon 4 times, until bead surface is residual oil removing electrolytic solution is not arranged;
(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
It is 25 ℃ that sensitizing is controlled temperature, and sensitization time is 2min, then pours out electrolytic solution, with distilled water, cleans glass microballon 4 times, until bead surface is residual sensitization electrolytic solution is not arranged;
(3), glass microballon activation, activation solution form and the content proportioning as follows
Palladous chloride 1g/L
Hydrochloric acid (content 37%) 15 mL/L
It is 2.5 that reactivation process is controlled pH, and temperature is 25 ℃, and soak time is 3min, then pours out electrolytic solution, with distilled water, cleans glass microballon 4 times, until bead surface is residual activated electrolyte is not arranged;
(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
Controlling pH in the chemical Ni-P plating process is 5.0, temperature is 85 ℃, after glass microballon is put into to plating solution, stir plating solution and make it to be uniformly dispersed, and stir in plating process discontinuous, intermittent time 5min, churning time 5min, plating time is 30min, after plating completes, pours out chemical plating fluid, after cleaning glass microballon 4 times with distilled water and be placed in loft drier and control temperature and be 25 ℃ and dried, finally in bead surface, form Ni-P alloy deposition layer
.
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 shown in Fig. 1 a, 85 ℃ of bath temperatures, the SEM pattern of bead surface coating during plating time 30min (amplifying 2000 times) is shown in Fig. 1 b.
By Fig. 1 a and Fig. 1 b, can be found out, glass microballon is after 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.Phenomenon in conjunction with observing in experiment illustrates that when bath temperature is high the glass microballon surface can not obtain satisfied Ni-P settled layer.
A kind of chemical plating Ni-P alloy technology of glass micro beads, comprise the steps:
(1), with embodiment 1;
(2), with embodiment 1;
(3), with embodiment 1;
(4), control temperature 60 C in the chemical Ni-P plating process, other conditions are with embodiment 1.
Glass microballon is put into to the plating solution discontinuous to be stirred while carrying out electroless plating, because electroless plating reaction speed at this temperature is moderate, therefore, all bead surface can form evenly, continuously, the Ni-P alloy deposition layer of light, there is no free metallic particles in plating solution 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, by Fig. 2 a and Fig. 2 b, drawn, glass microballon is when bath temperature is low after 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 glass microballon plates the glass microballon EDS spectrogram after the plating that in front and chemical Ni-P plating process, the control temperature is 60 ℃.Can show that from Fig. 3 and Fig. 4 electroless plating front glass bead surface element take O, Ca, Si, Na as main, the content of other element seldom.After electroless plating, bead surface element O, Si content descend, 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.EDS after the glass microballon electroless plating can also observe other element on spectrogram, and this is that electron beam is injected the place that coating is thinner, makes in spectrogram the element of the trace that has occurred that microballon itself is contained because the chemical Ni-P plating settled layer is thinner.
embodiment 3
A kind of chemical plating Ni-P alloy technology of glass micro beads, comprise 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
Sodium carbonate 10g/L
Sodium phosphate 30 g/L
OP-10 emulsifying agent 5 mL/L
It is 25 ℃ that ultrasonic procedure is controlled temperature, and time 3min, then pour out electrolytic solution, with distilled water, cleans glass microballon 4 times, until bead surface is residual oil removing electrolytic solution is not arranged;
(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
It is 25 ℃ that sensitizing is controlled temperature, and sensitization time is 2min, then pours out electrolytic solution, with distilled water, cleans glass microballon 4 times, until bead surface is residual sensitization electrolytic solution is not arranged;
(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
It is 2.0 that reactivation process is controlled pH, and temperature is 25 ℃, and soak time is 3min, then pours out electrolytic solution, with distilled water, cleans glass microballon 4 times, until bead surface is residual activated electrolyte is not arranged;
(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
Controlling pH in the chemical Ni-P plating process is 5.0, temperature is 50 ℃, after glass microballon is put into to plating solution, stir plating solution and make it to be uniformly dispersed, and stir in plating process discontinuous, intermittent time 10min, churning time 5min, plating time is 30min, after plating completes, pours out chemical plating fluid, after cleaning glass microballon 4 times with distilled water and be placed in loft drier and control temperature and be 25 ℃ and dried, finally in bead surface, form even, continuous, bright Ni-P alloy deposition layer
.
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, drawn by Fig. 5 a and Fig. 5 b, and glass microballon is when bath temperature is low after electroless plating, bead surface has coated even, the continuous settled layer of one deck, settled layer densification.
Fig. 6 is embodiment 3, controls when temperature is 50 ℃ the glass microballon EDS spectrogram after plating in glass microballon chemical Ni-P plating process.After electroless plating, bead surface element O, Si content descend as can be drawn from Figure 6, 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 chemical plating Ni-P alloy technology of glass micro beads, comprise 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
Sodium carbonate 12g/L
Sodium phosphate 32 g/L
OP-10 emulsifying agent 7mL/L
It is 25 ℃ that ultrasonic procedure is controlled temperature, and time 3min, then pour out electrolytic solution, with distilled water, cleans glass microballon 4 times, until bead surface is residual oil removing electrolytic solution is not arranged;
(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
It is 25 ℃ that sensitizing is controlled temperature, and sensitization time is 2min, then pours out electrolytic solution, with distilled water, cleans glass microballon 4 times, until bead surface is residual sensitization electrolytic solution is not arranged;
(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
It is 2.0 that reactivation process is controlled pH, and temperature is 25 ℃, and soak time is 3min, then pours out electrolytic solution, with distilled water, cleans glass microballon 4 times, until bead surface is residual activated electrolyte is not arranged;
(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
Controlling pH in the chemical Ni-P plating process is 5.0, temperature is 55 ℃, after glass microballon is put into to plating solution, stir plating solution and make it to be uniformly dispersed, and stir in plating process discontinuous, intermittent time 10min, churning time 5min, plating time is 30min, after plating completes, pours out chemical plating fluid, after cleaning glass microballon 4 times with distilled water and be placed in loft drier and control temperature and be 25 ℃ and dried, finally in bead surface, form even, continuous, bright Ni-P alloy deposition layer
.
In sum, solid glass micro-bead is through technique of the present invention, when the chemical plating fluid temperature is low, glass microballon in plating solution without agglomeration, can form even, continuous, fine and close Ni-P alloy deposition layer in bead surface, settled layer outward appearance light, in Ni-P alloy deposition layer, the content of Ni is 58.76～68.41% (wt), 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, within these modifications and change all belong to the scope of appended claims.
Claims (4)
1. a chemical plating Ni-P alloy technology of glass micro beads, controlling temperature in the electroless plating process is 50～60 ℃, plating time is 30min, it 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
Sodium carbonate 10～15g/L
Sodium phosphate 30～35g/L
OP-10 emulsifying agent 5～10mL/L
It is 20～30 ℃ that ultrasonic procedure is controlled temperature, and time 3min, then pour out the ultrasonic wave degreasing fluid, and cleaning glass microballon with distilled water does not have a ultrasonic wave degreasing fluid until bead surface is 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 to sensitization in sensitization electrolytic solution, and it is 20～30 ℃ that sensitizing is controlled temperature, and sensitization time is 2min, then pours out sensitization electrolytic solution, with distilled water clean glass microballon until bead surface not
Residual have sensitization electrolytic solution;
(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
Glass microballon after step (2) sensitization is processed to be inserted in activated electrolyte and activated, reactivation process controls pH and is 1.5～
2.5 temperature is 20～30 ℃, soak time is 3min, then pours out activated electrolyte, and cleaning glass microballon with distilled water does not have an activated electrolyte until bead surface is 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 activated processing in step (3) is inserted in chemical nickel phosphorus plating electrolytic solution and carried out electroless plating, and controlling pH in the chemical Ni-P plating process is 4.5～5.5, and temperature is 50～60 ℃, and plating time is 30min, rear with distilled water cleaning 3-4 time
And be placed in loft drier and control temperature and be 25 ℃ and dried, finally obtain the uniform glass microballon electroless plating of Ni-P settled layer
The Ni-P alloy.
2. a kind of chemical plating Ni-P alloy technology of glass micro beads as claimed in claim 1 is characterized in that: glass microballon ultrasonic wave oil removing in step (1), the ultrasonic wave degreasing fluid form and the content proportioning as follows:
Sodium hydroxide 10 g/L
Sodium carbonate 15 g/L
Sodium phosphate 35 g/L
OP-10 emulsifying agent 10 mL/L
It is 25 ℃ that ultrasonic procedure is controlled temperature, and time 3min, then pour out the ultrasonic wave degreasing fluid, and cleaning glass microballon with distilled water does not have a ultrasonic wave degreasing fluid until bead surface is residual;
Glass microballon sensitization in step (2), the proportioning of sensitization electrolytic solution composition and content thereof is as follows:
Tin protochloride 15 g/L
Hydrochloric acid 37% 100 mL/L
It is 25 ℃ that sensitizing is controlled temperature, and sensitization time is 2min, then pours out sensitization electrolytic solution, with distilled water, cleans glass microballon 4 times;
Glass microballon activation in step (3), activated electrolyte composition and content proportioning are as follows
Palladous chloride 1 g/L
Hydrochloric acid 37% 15 mL/L
It is 2.5 that reactivation process is controlled pH, and temperature is 25 ℃, and soak time is 3min, then pours out activated electrolyte, with distilled water, cleans glass microballon 4 times;
Glass microballon chemical Ni-P plating in step (4), the proportioning of chemical nickel phosphorus plating electrolytic solution 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
Controlling pH in the chemical Ni-P plating process is 5.0, temperature is 60 ℃, after glass microballon is put into to chemical nickel phosphorus plating electrolytic solution, stir chemical nickel phosphorus plating electrolytic solution and make it to be uniformly dispersed, and stir in plating process discontinuous, intermittent time 5min, churning time 5min, plating time is 30min, after plating completes, pours out chemical nickel phosphorus plating electrolytic solution, after cleaning glass microballon 4 times with distilled water and be placed in loft drier and control temperature and be 25 ℃ and dried, finally in bead surface, form Ni-P alloy deposition layer
.
3. a kind of chemical plating Ni-P alloy technology of glass micro beads as claimed in claim 1 is characterized in that: glass microballon ultrasonic wave oil removing in step (1), the ultrasonic wave degreasing fluid form and the content proportioning as follows:
Sodium hydroxide 5 g/L
Sodium carbonate 10 g/L
Sodium phosphate 30 g/L
OP-10 emulsifying agent 5 mL/L
It is 25 ℃ that ultrasonic procedure is controlled temperature, and time 3min, then pour out the ultrasonic wave degreasing fluid, with distilled water, cleans glass microballon 4 times, until bead surface is residual the ultrasonic wave degreasing fluid is not arranged;
Glass microballon sensitization in step (2), the proportioning of sensitization electrolytic solution composition and content thereof is as follows:
Tin protochloride 10 g/L
Hydrochloric acid 37% 50 mL/L
It is 25 ℃ that sensitizing is controlled temperature, and sensitization time is 2min, then pours out sensitization electrolytic solution, with distilled water, cleans glass microballon 4 times, until bead surface is residual sensitization electrolytic solution is not arranged;
Glass microballon activation in step (3), activated electrolyte composition and content proportioning are as follows:
Palladous chloride 0.5g/L
Hydrochloric acid 37% 10 mL/L
It is 2.0 that reactivation process is controlled pH, and temperature is 25 ℃, and soak time is 3min, then pours out activated electrolyte, with distilled water, cleans glass microballon 4 times, until bead surface is residual activated electrolyte is not arranged;
Glass microballon chemical Ni-P plating in step (4), the proportioning of chemical nickel phosphorus plating electrolytic solution 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
Controlling pH in the chemical Ni-P plating process is 5.0, temperature is 50 ℃, after glass microballon is put into to chemical nickel phosphorus plating electrolytic solution, stirring chemical nickel phosphorus plating electrolytic solution makes it to be uniformly dispersed, and stir in plating process discontinuous, intermittent time 10min, churning time 5min, plating time is 30min, after completing, plating pours out chemical nickel phosphorus plating electrolytic solution, after cleaning glass microballon 4 times with distilled water and be placed in loft drier and control temperature and be 25 ℃ and dried, finally in bead surface, form Ni-P alloy deposition layer
.
4. a kind of chemical plating Ni-P alloy technology of glass micro beads as claimed in claim 1 is characterized in that: glass microballon ultrasonic wave oil removing in step (1), the ultrasonic wave degreasing fluid form and the content proportioning as follows:
Sodium hydroxide 8.5 g/L
Sodium carbonate 12 g/L
Sodium phosphate 32 g/L
OP-10 emulsifying agent 7mL/L
It is 25 ℃ that ultrasonic procedure is controlled temperature, and time 3min, then pour out the ultrasonic wave degreasing fluid, with distilled water, cleans glass microballon 4 times, until bead surface is residual the ultrasonic wave degreasing fluid is not arranged;
Glass microballon sensitization in step (2), the proportioning of sensitization electrolytic solution composition and content thereof is as follows:
Tin protochloride 12 g/L
Hydrochloric acid 37% 75 mL/L
It is 25 ℃ that sensitizing is controlled temperature, and sensitization time is 2min, then pours out sensitization electrolytic solution, with distilled water, cleans glass microballon 4 times, until bead surface is residual sensitization electrolytic solution is not arranged;
Glass microballon activation in step (3), activated electrolyte composition and content proportioning are as follows:
Palladous chloride 0.8 g/L
Hydrochloric acid 37% 12 mL/L
It is 2.0 that reactivation process is controlled pH, and temperature is 25 ℃, and soak time is 3min, then pours out activated electrolyte, with distilled water, cleans glass microballon 4 times, until bead surface is residual activated electrolyte is not arranged;
Glass microballon chemical Ni-P plating in step (4), the proportioning of chemical nickel phosphorus plating electrolytic solution 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
Controlling pH in the chemical Ni-P plating process is 5.0, temperature is 55 ℃, after glass microballon is put into to chemical nickel phosphorus plating electrolytic solution, stirring chemical nickel phosphorus plating electrolytic solution makes it to be uniformly dispersed, and stir in plating process discontinuous, intermittent time 10min, churning time 5min, plating time is 30min, after completing, plating pours out chemical nickel phosphorus plating electrolytic solution, after cleaning glass microballon 4 times with distilled water and be placed in loft drier and control temperature and be 25 ℃ and dried, finally in bead surface, form Ni-P alloy deposition layer
.
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| CN104018139B (en) * | 2014-06-20 | 2016-04-13 | 哈尔滨工业大学 | A kind of preparation method of cenosphere/Ni-Fe-P/Cu composite deposite |
| CN104018143B (en) * | 2014-06-20 | 2016-04-13 | 哈尔滨工业大学 | A kind of method of cenosphere surface chemistry plating amorphous Ni-Fe-P |
| CN105112891A (en) * | 2015-09-02 | 2015-12-02 | 昆明理工大学 | Method for chemically plating surface of diamond with Ni and P in microwave-ultrasound combined mode |
| CN106512874B (en) * | 2015-09-09 | 2019-04-12 | 中国科学院理化技术研究所 | A kind of method of glass hollow microsphere surface coating spinelle type ferrite shell and the hollow complex microsphere of gained and application |
| CN107958946A (en) * | 2017-11-17 | 2018-04-24 | 扬州乾照光电有限公司 | A kind of light-emitting diode chip for backlight unit for improving current expansion and preparation method thereof |
| 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 |
| 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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