CN104098277A - Method for copperizing and silvering on surface of glass bead, and copperized and silvered glass bead - Google Patents
Method for copperizing and silvering on surface of glass bead, and copperized and silvered glass bead Download PDFInfo
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- CN104098277A CN104098277A CN201410334422.2A CN201410334422A CN104098277A CN 104098277 A CN104098277 A CN 104098277A CN 201410334422 A CN201410334422 A CN 201410334422A CN 104098277 A CN104098277 A CN 104098277A
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- glass microballon
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Abstract
The invention discloses a method for copperizing and silvering on the surface of a glass bead. The method comprises the steps that 1) alkaline cleaning and coarsening pretreatment is performed; 2) sensitizing treatment is performed on the glass bead by a sensitizing solution; 3) reduction copperizing treatment is performed on the glass bead by a reduction solution in a copperizing solution; and 4) replacement silvering treatment is performed on the copperized glass bead by a silver ammonia solution in a silvering solution, and then the copperized and silvered glass bead in a double-layer structure is obtained. The volume resistivity of the glass bead is less than or equal to 10<-3>omega.cm; the glass bead has the characteristics of uniform plating, low density, good conductivity, good storage capability and the like; and the method is suitable for preparing conductive compounds such as conductive rubber, a conductive coating and a conductive adhesive.
Description
Technical field
The present invention relates to a kind of preparation method of electromagnetic shielding material, be specifically related to a kind of silver-plated method of copper facing of carrying out on glass microballon surface, the invention still further relates to a kind of copper facing silvered glass microballon obtained by this method.
Background technology
Along with the development of electronic industry, the various electrical equipments such as computer, information processing device, electronic communication equipment as the carrier of information technology in industry-by-industry widespread use, bring great convenience to the mankind, but the electromagnetic radiation that equipment produces, electromagnetic pollution become very important social concern.Reach excellent effectiveness of shielding because conductive material can rely on high frequency band reflection electromagnetic wave, therefore adopting conductive rubber and electroconductive binder is the effective means that prevents electromagnetic radiation pollution.Aspect shielding electromagnetic interference, conductive rubber and electroconductive binder also can be filled the gap of electronics, instrument, and can connect the device such as EMI shielding window, ventilation waveguide.
At present, the kind of conductive compound (tackiness agent) mainly contains gold system, silver system, copper system, the silver-plated system of copper, graphite system, graphite nickel plating system etc., considers electroconductibility, scale resistance and price factor, and silver system, the silver-plated system of copper are most widely used.There is good conductivity, feature that scale resistance is good using silver system as the conductive compound of conductive filler material, but because silver particles migration and expensive reason have limited its use range.Conductive compound good conductivity using copper system as filler, but resistance to oxidation poor stability, along with the easy oxidation of increase copper powder of time finally becomes isolator.In order to overcome these shortcomings; in prior art; as disclosed the preparation method of silver-plated copper powder in CN1049622A and CN1130553A, the method is utilized silver-colored resistance to oxidation and stable feature, has retained the electroconductibility of copper; by after copper powder degreasing; remove copper oxide film with acid, then add silver salt solution, make copper displacement silver ions; allow deposition of silver on Copper Powder Surface, form layer protective layer, make the conductive copper powder that scale resistance is good.The conductive rubber of preparing with this copper silvering powder and tackiness agent good conductivity, scale resistance is good, price is more silver-colored is that powder significantly reduces.But it is that density is large that silver powder, copper silvering powder have a common shortcoming, in tackiness agent, these powder loading levels are high, the 75%-85% left and right that accounts for gross weight, causes final electromagnetic shielding material conductive rubber and electroconductive binder density to increase, and has increased the use cost of material.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of silver-plated method of copper facing of carrying out on glass microballon surface is provided, the copper facing silvered glass microballon making by the method, has the advantages that density is little, silver content is low, conduct electricity very well.
For achieving the above object, the present invention is by the following technical solutions:
In the silver-plated method of glass microballon copper coating, comprise the following steps:
1) alligatoring: glass microballon is placed in to etching reagent, at 10～60 DEG C, slowly stirs after 15～45 minutes and filter, and clean extremely neutral for subsequent use with clear water;
2) sensitization: the glass microballon after roughening treatment is placed in to sensitizing solution, and sensitization is processed after 5～30 minutes and filtered at 15～60 DEG C, and for subsequent use after extremely neutral with clear water cleaning;
3) reduction copper facing: the glass microballon after sensitization is placed in to copper plating solution, adds reduced liquid under agitation condition, and reduce copper plating treatment and filter after 5～30 minutes at 30～70 DEG C, and clean to for subsequent use with water seal after neutrality with clear water;
4) replacement ag plating: the glass microballon after copper facing is placed in to silver plating solution, adds silver ammino solution under agitation condition, and replace silver plating reaction and filter after 5～40 minutes at 30～60 DEG C, and clean to neutrality and dry at 50～80 DEG C with clear water.
Preferably: before described alligatoring step, also comprise removal step, described removal step is: glass microballon is placed in to alkali lye, and at 30～60 DEG C, stir process was filtered after 10～50 minutes, and with clear water cleaning extremely neutrality is for subsequent use.
Preferably: described alkali lye is NaOH or KOH solution, and its concentration is 10～50wt%.
Preferably: described etching reagent is hydrofluoric acid solution, its concentration is 3～30wt%.
Preferably: described sensitizing solution is the mixed solution of stannous chloride solution and hydrochloric acid soln, wherein, the concentration of stannous chloride solution is 5～15g/L, and the concentration of hydrochloric acid solution is 20ml～80ml/L.
Preferably: in 1L, the consisting of of described copper plating solution: copper sulfate: 20～120g, EDTA and/or EDETATE SODIUM: 40～150g, Seignette salt and/soluble tartrate: 50～150g, ammoniacal liquor: 10～60, sodium hydroxide and/or potassium hydroxide: 1～10g, distilled water: surplus.
Preferably: described reduced liquid is aldehydes or carbohydrate.
Preferably: described aldehydes is 99% formaldehyde solution, by required copper facing amount, its consumption is 50～120ml/L, and described carbohydrate is 50% glucose solution, and by required copper facing amount, its consumption is 75～180ml/L.
Preferably: in 1L, the consisting of of described silver plating solution: EDTA and/or EDETATE SODIUM: 40～150g, Seignette salt and/or soluble tartrate: 10～80g, sodium hydroxide and/or potassium hydroxide 1～10g/L, distilled water: surplus.
The copper facing silvered glass microballon being made by aforesaid method, its inner core is that particle diameter is the hollow or solid glass micro-bead of 5～100 μ m, its surface is coated with successively copper coating and silvering outside interior.
Beneficial effect of the present invention is: the copper facing silvered glass microballon 1) making by method of the present invention, and its surperficial silvered film weight only accounts for the 5-15% of gross weight, makes into silver-plated copper powder cost and greatly reduces, and is convenient to industrial mass production and uses; 2) show according to data document: the tap density of silver powder is 10.4g/cm
3, the tap density of copper powder is 8.7g/cm
3, the tap density > 8.7g/cm of copper silvering powder
3, and copper facing silvered glass microballon tap density provided by the present invention is < 8.7g/cm
3, can effectively reduce the weight of goods; 3) copper facing silvered glass microballon has the good electric conductivity of copper silvering powder, volume specific resistance≤10
-3Ω cm, and due to the low specific surface area of spherical glass microballon, thereby only need less silver can be coated copper facing glass microballon completely, and make the copper facing silvered glass microballon making there is relatively low density, therefore reduce material cost and use cost; 4) have a storage stability good, the features such as good heat resistance, are applicable to prepare the conducting material such as conductive rubber, electrically conducting coating and electroconductive binder.
Embodiment
Below in conjunction with specific embodiment, the specific embodiment of the present invention is described further.But the present invention is not limited in following embodiment.Unless otherwise noted, each raw material of the present invention all can be bought and can be obtained by market.
Carry out the silver-plated method of copper facing on glass microballon surface, the particle diameter of described glass microballon is 5～100 μ m preferably, comprise the following steps:
1) removal of impurities: glass microballon is placed in to alkali lye, at 30～60 DEG C, stir process was filtered after 10～50 minutes, and cleaned to neutral for subsequent use with clear water, to remove the impurity such as greasy dirt on glass microballon surface, wherein, described alkali lye is that concentration is NaOH or the KOH solution of 10～50wt%;
2) alligatoring: with etching reagent, roughening treatment is carried out in glass microballon surface, described roughening treatment process is: glass microballon is placed in to etching reagent, at 10～60 DEG C, slowly stirs after 15～45 minutes and filter, and clean extremely neutral for subsequent use with clear water; Wherein, the preferred hydrofluoric acid solution of described etching reagent, its concentration is 3～30wt%;
3) sensitization: the glass microballon after roughening treatment is placed in to sensitizing solution, and sensitization is processed after 5～30 minutes and filtered at 15～60 DEG C, and for subsequent use after extremely neutral with clear water cleaning; Wherein, described sensitizing solution is the mixed solution of stannous chloride solution and hydrochloric acid soln, wherein, and tin protochloride (SnCl
22H
2o) concentration of solution is 5～15g/L, and the concentration of hydrochloric acid (HCl, 37%) solution is 20ml～80ml/L;
4) reduction copper facing: the glass microballon after sensitization is placed in to copper plating solution, under agitation condition, add reduced liquid, and at 30～70 DEG C, reduce copper plating treatment 5～30 minutes, copper plating solution reacts with reduced liquid, the copper of reduction is deposited on glass microballon, forms copper pre-plating layer; Then filter, and clean to for subsequent use with water seal after neutrality with clear water; Wherein, in 1g glass microballon, the consumption of copper plating solution is 12.5～35.5ml, and in every liter of copper plating solution, it consists of: copper sulfate (CuSO
45H
2o): 20～120g, EDTA and/or EDETATE SODIUM: 40～150g, Seignette salt and/soluble tartrate: 50～150g, ammoniacal liquor: 10～60, sodium hydroxide and/or potassium hydroxide: 1～10g, distilled water: surplus; Described reduced liquid is aldehydes or carbohydrate, wherein, and the preferred formaldehyde of described aldehydes (99%) solution, by required copper facing amount, its consumption is 50～120ml/L, the preferred glucose solution of described carbohydrate (50%), by required copper facing amount, its consumption is 75～180ml/l; The thickness of coating of copper can be by Cu in copper plating solution
2+content determine, when copper plating solution be glass microballon weight 20%～120% time, in glass microballon, the content of copper is 5%～40%;
5) replacement ag plating: the glass microballon after copper facing is placed in to silver plating solution, adds silver ammino solution under agitation condition, and replace silver plating reaction and filter after 5～40 minutes at 30～60 DEG C, and clean to neutrality and dry at 50～80 DEG C with clear water; Wherein, in the initial glass microballon of 1g, the consumption of silver plating solution is: 5g～15g; In every liter of silver plating solution, it consists of: EDTA and/or EDETATE SODIUM: 40～150g, Seignette salt and/or soluble tartrate: 10～80g, sodium hydroxide and/or potassium hydroxide 1～10g, distilled water: surplus; Consisting of of described silver ammino solution: in every 200ml silver ammino solution, Silver Nitrate 7～24g, ammoniacal liquor 50～170ml, distilled water: surplus.
Embodiment 1
Taking preparation copper facing amount 20wt%, silver-plated amount as 5wt% glass microballon is as example, its preparation method comprises the following steps:
1) removal of impurities: the glass microballon that is 30 μ m by 80g particle diameter is placed in the NaOH solution that 200ml concentration is 30wt%, stir process 20 minutes at 40 DEG C, to remove the impurity such as greasy dirt on glass microballon surface, then filter and clean to for subsequent use after neutral with clear water;
2) alligatoring: glass microballon after treatment removal of impurities is placed in to the hydrofluoric acid solution that 100ml concentration is 20wt%, and the speed stirring with 100rp at 35 DEG C was filtered after 15 minutes, and cleaned to neutral for subsequent use with clear water;
3) sensitization: the glass microballon after roughening treatment is placed in to the sensitizing solution of 500ml, sensitization is processed after 20 minutes and filtered at 30 DEG C, and for subsequent use after extremely neutral with clear water cleaning; Wherein, described sensitizing solution is that concentration is the tin protochloride of 10g/L and the mixed solution of the hydrochloric acid soln that concentration is 60ml/L;
4) reduction copper facing: the glass microballon after sensitization is placed in to the copper plating solution of 1L, adds reduced liquid under agitation condition, and reduce copper plating treatment and filter after 20 minutes at 55 DEG C, and clean to for subsequent use with water seal after neutrality with clear water; Wherein, in 1L copper plating solution, it consists of: copper sulfate (CuSO
45H
2o): 78g, EDETATE SODIUM: 80g, Seignette salt: 76g, ammoniacal liquor: 40ml, sodium hydroxide: 4.5g, distilled water: surplus; Described reduced liquid is formaldehyde (99%) solution, and by required copper facing amount, the consumption of described formaldehyde (99%) solution is 45ml/L;
5) replacement ag plating: the glass microballon after copper facing is placed in to 800ml silver plating solution, under agitation condition, add silver ammino solution, and at 30 DEG C, replace silver plating reaction and filter after 20 minutes, and clean to neutrality and at 65 DEG C, dry and obtain copper facing silvered glass microballon of the present invention with clear water; Wherein, consisting of of every liter of silver plating solution: EDETATE SODIUM: 100g, Seignette salt: 50g, sodium hydroxide 5g, distilled water: surplus; Consisting of of described silver ammino solution: in every 200ml silver ammino solution, Silver Nitrate is 7.8g, and ammoniacal liquor is 12ml, distilled water: surplus.
Embodiment 2
Taking the glass microballon of preparation copper facing amount 40wt% silver-plated 8wt% as example, described preparation method comprises the following steps:
1) removal of impurities: the glass microballon that is 30 μ m by 60g particle diameter is placed in the NaOH solution that 200ml concentration is 30wt%, stir process 20 minutes at 40 DEG C, to remove the impurity such as greasy dirt on glass microballon surface, then filter and clean to for subsequent use after neutral with clear water;
2) alligatoring: glass microballon after treatment removal of impurities is placed in to the hydrofluoric acid solution that 100ml concentration is 20wt%, and the speed stirring with 100rp at 35 DEG C was filtered after 15 minutes, and cleaned to neutral for subsequent use with clear water;
3) sensitization: the glass microballon after roughening treatment is placed in to the sensitizing solution of 500ml, sensitization is processed after 20 minutes and filtered at 30 DEG C, and for subsequent use after extremely neutral with clear water cleaning; Wherein, described sensitizing solution is that concentration is the tin protochloride of 10g/L and the mixed solution of the hydrochloric acid soln that concentration is 60ml/L;
4) reduction copper facing: the glass microballon after sensitization is placed in to the copper plating solution of 2L, adds reduced liquid under agitation condition, and reduce copper plating treatment and filter after 20 minutes at 55 DEG C, and clean to for subsequent use with water seal after neutrality with clear water; Wherein, consisting of of every liter of copper plating solution: copper sulfate (CuSO
45H
2o): 78g, EDETATE SODIUM: 80g, Seignette salt: 76g, ammoniacal liquor: 40ml, sodium hydroxide: 4.5g, distilled water: surplus; By required copper facing amount, the consumption of described formaldehyde (99%) solution is 100ml/L;
5) replacement ag plating: the glass microballon after copper facing is placed in to 800ml silver plating solution, under agitation condition, add silver ammino solution, and at 30 DEG C, replace silver plating reaction and filter after 30 minutes, and clean to neutrality and at 60 DEG C, dry and obtain copper facing silvered glass microballon of the present invention with clear water; Wherein, consisting of of every liter of silver plating solution: EDETATE SODIUM: 110g; Seignette salt: 60g, sodium hydroxide 6g, distilled water: surplus; Described silver ammino solution, it consists of: in every 200ml silver ammino solution, Silver Nitrate is 12.4g, and ammoniacal liquor is 20ml, distilled water: surplus.
The glass microballon that embodiment 1 and 2 is made carries out density and conducting performance test, and its test result is as shown in table 1, and wherein, the testing method of resistance is: YST587.6-2006; The testing method of tap density is GB/T5162-2006.
Table 1 glass microballon the performance test results
| ? | Copper content (%) | Silver content (%) | Powder resistance (m Ω cm) | Tap density (g/cm 3) |
| Embodiment 1 | 20 | 5 | 0.9 | 1.38 |
| Embodiment 2 | 40 | 8 | 0.7 | 1.51 |
As can be seen from Table 1, adopt the prepared glass microballon of the present invention, the per-cent that its surperficial silvered film weight accounts for gross weight is low, and silver-plated copper powder cost is greatly reduced, and is convenient to industrial mass production and uses.And, the double-deck copper facing silvered glass microballon making, its volume specific resistance≤10
-3Ω cm, have that coating is even, density is little, electroconductibility and the good feature of storage characteristics, the thickness of pre-copper plate has determined the conductive layer that glass microballon is final, in the time that copper plate is thinner, its conductivity is slightly better than silvered glass microballon, in the time that thickness of coated copper layer is thicker, its conductivity is equivalent to copper facing silver glass microballon.Be applicable to prepare the compounds such as conductive rubber, wire coating and electroconductive binder.
Specific embodiment described in the invention is only for the detailed description to copper facing silvered glass preparation of microbeads specific implementation process, instead of for the concrete restriction to its preparation method.Any modification that this method is carried out and improvement, the substituting and using of similar or close material in the scope of the claims or category, all belongs to scope of patent protection of the present invention.
Claims (10)
1. in the silver-plated method of glass microballon copper coating, it is characterized in that: comprise the following steps:
1) alligatoring: glass microballon is placed in to etching reagent, at 10～60 DEG C, slowly stirs after 15～45 minutes and filter, and clean extremely neutral for subsequent use with clear water;
2) sensitization: the glass microballon after roughening treatment is placed in to sensitizing solution, and sensitization is processed after 5～30 minutes and filtered at 15～60 DEG C, and for subsequent use after extremely neutral with clear water cleaning;
3) reduction copper facing: the glass microballon after sensitization is placed in to copper plating solution, adds reduced liquid under agitation condition, and reduce copper plating treatment and filter after 5～30 minutes at 30～70 DEG C, and clean to for subsequent use with water seal after neutrality with clear water;
4) replacement ag plating: the glass microballon after copper facing is placed in to silver plating solution, adds silver ammino solution under agitation condition, and replace silver plating reaction and filter after 5～40 minutes at 30～60 DEG C, and clean to neutrality and dry at 50～80 DEG C with clear water.
2. method according to claim 1, it is characterized in that: before described alligatoring step, also comprise removal step, described removal step is: glass microballon is placed in to alkali lye, and at 30～60 DEG C, stir process was filtered after 10～50 minutes, and cleans extremely neutral for subsequent use with clear water.
3. method according to claim 2, is characterized in that: described alkali lye is NaOH or KOH solution, and its concentration is 10～50wt%.
4. method according to claim 1, is characterized in that: described etching reagent is hydrofluoric acid solution, and its concentration is 3～30wt%.
5. method according to claim 1, is characterized in that: described sensitizing solution is the mixed solution of stannous chloride solution and hydrochloric acid soln, and wherein, the concentration of stannous chloride solution is 5～15g/L, and the concentration of hydrochloric acid soln is 20ml～80ml/L.
6. method according to claim 1, it is characterized in that: in 1L, consisting of of described copper plating solution: copper sulfate: 20～120g, EDTA and/or EDETATE SODIUM: 40～150g, Seignette salt and/soluble tartrate: 50～150g, ammoniacal liquor: 10～60, sodium hydroxide and/or potassium hydroxide: 1～10g, distilled water: surplus.
7. method according to claim 1, is characterized in that: described reduced liquid is aldehydes or carbohydrate.
8. method according to claim 7, is characterized in that: described aldehydes is 99% formaldehyde solution, and by required copper facing amount, its consumption is 50～120ml/L, and described carbohydrate is 50% glucose solution, and by required copper facing amount, its consumption is 75～180ml/L.
9. method according to claim 1, it is characterized in that: in 1L, the consisting of of described silver plating solution: EDTA and/or EDETATE SODIUM: 40～150g, Seignette salt and/or soluble tartrate: 10～80g, sodium hydroxide and/or potassium hydroxide 1～10g/L, distilled water: surplus.
10. the copper facing silvered glass microballon being made by the method described in claim 1 or 2, is characterized in that: its inner core is that particle diameter is the hollow or solid glass micro-bead of 5～100 μ m, and its surface is coated with copper coating and silvering from the inside to the outside successively.
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|---|---|---|---|
| CN201410334422.2A CN104098277B (en) | 2014-07-14 | 2014-07-14 | Method for copperizing and silvering on surface of glass bead, and copperized and silvered glass bead |
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| CN108504152A (en) * | 2018-05-07 | 2018-09-07 | 合肥仁德电子科技有限公司 | The high heat radiation coating of a kind of electronic equipment shell |
| CN109810462A (en) * | 2018-12-27 | 2019-05-28 | 会通新材料股份有限公司 | A kind of bloom cubic texture material and preparation method thereof |
| CN111138706A (en) * | 2020-01-08 | 2020-05-12 | 四川大学 | Polymer electromagnetic shielding composite foam with gradient filler structure and preparation method thereof |
| CN111377617A (en) * | 2020-04-09 | 2020-07-07 | 西安工程大学 | Preparation method of hollow glass bead surface silver plating |
| CN113278219A (en) * | 2021-05-07 | 2021-08-20 | 广东力王新材料有限公司 | Self-temperature-control heating sheet and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108504152A (en) * | 2018-05-07 | 2018-09-07 | 合肥仁德电子科技有限公司 | The high heat radiation coating of a kind of electronic equipment shell |
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| CN113278219A (en) * | 2021-05-07 | 2021-08-20 | 广东力王新材料有限公司 | Self-temperature-control heating sheet and preparation method thereof |
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Effective date of registration: 20180522 Address after: 402760 No. 1-2, 3rd floor, F07 building, electroplating concentrated processing area, Bishan Industrial Park, Chongqing. Patentee after: Chongqing New Fortune Technology Co., Ltd. Address before: 200030 395 room, No. 9818, No. 1, Hu min Road, Xuhui District, Shanghai Patentee before: SHANGHAI QIWEI NEW MATERIAL TECHNOLOGY CO., LTD. |
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