CN106270545A - A kind of high-tap density noble metal raw powder's production technology - Google Patents
A kind of high-tap density noble metal raw powder's production technology Download PDFInfo
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- CN106270545A CN106270545A CN201510338396.5A CN201510338396A CN106270545A CN 106270545 A CN106270545 A CN 106270545A CN 201510338396 A CN201510338396 A CN 201510338396A CN 106270545 A CN106270545 A CN 106270545A
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Abstract
The invention discloses a kind of high-tap density noble metal raw powder's production technology, comprise the following steps: (1) prepares precious metal salt solution and reductant solution respectively；(2) in reductant solution, add macromolecule dispersing agent and the polymerization inhibitor of precious metal salt weight 0-5% of precious metal salt weight 5-50%；(3) under agitation precious metal salt solution is joined in the reductant solution of step 2 gained；(4) above-mentioned solution be stirred continuously and ensure to react and fully carry out, backward reaction system in add surface modifier, powder surface is modified；(5), after powder body centrifugation or powder natural subsidence, clean for several times with deionized water；(6) dry and beat powder and disperse and get final product.The high-tap density noble metal raw powder's production technology of the present invention can not only realize batch production, and the powder dispersity prepared is good, and tap density is higher.
Description
Technical field
The present invention relates to a kind of noble metal raw powder's production technology, the preparation side of a kind of high-tap density noble metal powder body
Method.
Background technology
Precious Metal is the most important material of electronics industry, along with miniaturization, miniaturization and the micro-nano skill of electronic product
The development of art, prepares various conductive thick film slurry with precious metal powder body and is widely used in coating and the electricity of printed circuit
Road connects mutually, and the printed resolution of Precious Metal is limited by the performance parameter of noble metal powder body greatly.The nearest
The extensive application of LTCC technology and developing rapidly over Nian, then has higher requirement to noble metal powder body, and your gold it requires
The features such as it is high that genus powder body has tap density, good dispersion, so just can further promote the bullion content in slurry also
Obtain higher printed resolution.The method preparing at present noble metal powder body both at home and abroad is a lot, including vapor phase method, solid phase method,
Liquid phase method etc..Wherein the investment of vapor phase method is big, energy consumption is high, productivity is low；Diameter of particle prepared by solid phase method is bigger than normal；Liquid phase method
Technique is relatively easy, is suitable for large batch of industrialized production.
There is the problem such as particle agglomeration, bad dispersibility in the noble metal powder body that domestic enterprise produces at present, the slurry prepared exists
Sintering shrinkage is big, and film layer is the finest and close, thus is not suitable for the high-end field such as LTCC technology, solaode.And these
The specific requirement of noble metal powder body is by field: monodispersity is good, and powder reuniting is few, and tap density is high and specific surface area is little.
Summary of the invention
The purpose of the present invention is contemplated to overcome above-mentioned technological difficulties to provide a kind of high-tap density, single dispersing, specific surface area
Little and be prone to the noble metal raw powder's production technology of large-scale production.
For achieving the above object, the present invention provides following technical scheme:
A kind of high-tap density noble metal raw powder's production technology, comprises the following steps:
(1) preparing precious metal salt solution and reductant solution respectively, precious metal salt solution concentration is 1-200g/L, reducing agent
Solution concentration is 1-200g/L；
(2) in described reductant solution, add macromolecule dispersing agent and polymerization inhibitor, and make it fully dissolve, mix all
Even；
(3) under agitation described precious metal salt solution is joined in step (2) in the reductant solution of gained；
(4) above-mentioned solution be stirred continuously and ensure to react and fully carry out, backward reaction system in add surface modification
Agent, is modified powder surface；
(5) after powder body centrifugation or powder natural subsidence, with deionized water and alcohol washes for several times；
(6) dry under the conditions of 50-100 DEG C, play powder dispersion, obtain the average particle size distribution expensive gold of high jolt ramming in 1-3 μm
Belong to powder body.
As the further scheme of the present invention: described precious metal salt be gold chloride, silver nitrate, Palladous nitrate., dichloro two ammino palladium,
One in chloroplatinic acid.
As the present invention further scheme: described macromolecule dispersing agent is polyvinylpyrrolidone, polyvinyl alcohol, gelatin
With a kind of or the most several mixture in arabic gum.
As the present invention further scheme: described polymerization inhibitor is in Colophonium, acrylic resin and polyvinyl butyral resin
Or the most several a kind of mixture.
As the present invention further scheme: the weight of described macromolecule dispersing agent is the 5-50% of precious metal salt.
As the present invention further scheme: the weight of described polymerization inhibitor is the 0-5% of precious metal salt.
As the present invention further scheme: in described step (3), described reducing agent and the mass ratio of precious metal salt
It is 1: 1.
As the present invention further scheme: described reducing agent be ascorbic acid, formaldehyde, sodium hypophosphite, hydrazine hydrate,
A kind of or the most several mixture of sodium sulfite.
As the present invention further scheme: described surface modifier be stearic acid, caproic acid, enanthic acid, octanoic acid, n-nonanoic acid,
Hexadecanol, lauryl mercaptan, butyl stearate, a kind of or the most several mixture of ethyl caprilate.
Compared with prior art, the invention has the beneficial effects as follows: reactions steps of the present invention is simple, be suitable for extensive batch
Produce；Additionally by the adjustment of concentration, reaction temperature, powder parameters can be carried out controlled adjustment；The present invention introduces in the reaction
Metal surface modification step so that powder surface is changed into oil-wetted surface by hydrophilic, is allowed in the later stage slurry operation of rolling more
Easily it is sufficiently mixed with the oil-based solvent in organic carrier；Noble metal powder body prepared by the present invention takes into account dispersibility, degree of crystallinity
And tap density, the application requirement of used in electronic industry noble metal powder body can be met.
Accompanying drawing explanation
Fig. 1 is the SEM figure of high-tap density noble metal raw powder's production technology gained argentum powder.
Fig. 2 is the grain size distribution of high-tap density noble metal raw powder's production technology gained argentum powder.
Fig. 3 is the SEM figure of high-tap density noble metal raw powder's production technology gained bronze.
Fig. 4 is the grain size distribution of high-tap density noble metal raw powder's production technology gained palladium powder.
Fig. 5 is the grain size distribution of high-tap density noble metal raw powder's production technology gained gained platinum powder.
Detailed description of the invention
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clearly and completely
Describe, it is clear that described embodiment is only a part of embodiment of the present invention rather than whole embodiments.Based on this
Embodiment in invention, the every other reality that those of ordinary skill in the art are obtained under not making creative work premise
Execute example, broadly fall into the scope of protection of the invention.
Embodiment 1:
Compound concentration is the vitamin C reducing solution 1L of silver nitrate solution 1L and 200g/L of 200g/L respectively, and to reduction
Liquid adds 500mL concentration and is the gelatin dispersant solution of 200g/L and 5mL concentration is the polyvinyl butyral resin of 1g/mL
Solution, to add the reductant solution after dispersant as mother solution, will silver nitrate solution stir under be added dropwise in mother-liquor,
Continue stirring 5-10min after having fed, treat that powder body color no longer changes addition 1g ethyl caprilate in backward reaction system, it
Rear standing sedimentation；Cleaning with deionized water after precipitating 3-5 time, 60 DEG C of dry powder body, gained argentum powder is as it is shown in figure 1, have
The most spherical, its particle diameter is distributed as in figure 2 it is shown, D50 is 2.3 μm, good dispersion, narrow diameter distribution, tap density
6.0g/mL。
Embodiment 2:
Compound concentration is the vitamin C reducing solution 1L of chlorauric acid solution 1L and 100g/L of 100g/L respectively, and to reduction
Adding 500mL concentration in liquid is the polyvinyl alcohol dispersant solution of 20g/L, to add the reductant solution after dispersant as mother
Liquid, adds chlorauric acid solution in mother-liquor under stirring in 5s, continues stirring 5-10min, treat powder body after having fed
Color no longer changes addition 0.5g stearic acid, afterwards standing sedimentation in backward reaction system；Precipitation 3-5 is cleaned with deionized water
After secondary, 60 DEG C of dry powder body, gained bronze is as it is shown on figure 3, have the most spherical, and D50 is 1.7 μm, good dispersion,
Narrow diameter distribution, tap density 8.1g/mL.
Embodiment 3:
Compound concentration is the sodium hypophosphite reducing solution 1L of palladium nitrate solution 1L and 200g/L of 200g/L respectively, and to also
Stock solution adds 160mL concentration and is the polyvinylpyrrolidone dispersant solution of 200g/L and 3mL concentration is the third of 1g/mL
Olefin(e) acid resin solution, to add the reductant solution after dispersant as mother solution, is added dropwise to palladium nitrate solution under stirring also
In original nut liquid, after having fed, continue stirring 5-10min, treat that powder body color no longer changes addition 1g ten in backward reaction system
Six alcohol, afterwards standing sedimentation；Clean after precipitating 3-5 time with deionized water, 60 DEG C of dry powder body, gained palladium powder footpath is distributed
As shown in Figure 4, D50 is 1.4 μm, good dispersion, narrow diameter distribution, tap density 5.6g/mL.
Embodiment 4:
Compound concentration is platinum acid chloride solution 1L and the 200g hydrazine hydrate reduction liquid of 200g/L respectively, and adds in reducing solution
100mL concentration is the polyvinylpyrrolidone dispersant solution of 100g/L.With the reductant solution after addition dispersant as mother
Liquid, is added dropwise over platinum acid chloride solution in mother-liquor under stirring, continues stirring 5-10min, treat powder body face after having fed
Color no longer changes addition 0.5g lauryl mercaptan, afterwards standing sedimentation in backward reaction system；The most clear with deionized water and ethanol
Washing after precipitating 3-5 time, 60 DEG C of dry powder body, gained platinum powder particle diameter is distributed as it is shown in figure 5, D50 is 1.3 μm, dispersibility
Good, narrow diameter distribution, tap density 4.9g/mL.
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, and do not carrying on the back
In the case of the spirit or essential attributes of the present invention, it is possible to realize the present invention in other specific forms.Therefore, no matter from
From the point of view of which point, all should regard embodiment as exemplary, and be nonrestrictive, the scope of the present invention is by appended power
Profit requires rather than described above limits, it is intended that all by fall in the implication of equivalency and scope of claim
Change is included in the present invention.Should not be considered as limiting involved claim by any reference in claim.
Although moreover, it will be appreciated that this specification is been described by according to embodiment, but the most each embodiment only comprises
One independent technical scheme, this narrating mode of description is only the most for clarity sake, and those skilled in the art should be by
Description is as an entirety, and the technical scheme in each embodiment can also be through appropriately combined, and forming those skilled in the art can
With other embodiments understood.
Claims (9)
1. a high-tap density noble metal raw powder's production technology, it is characterised in that comprise the following steps:
(1) preparing precious metal salt solution and reductant solution respectively, precious metal salt solution concentration is 1-200g/L, reducing agent
Solution concentration is 1-200g/L；
(2) in described reductant solution, add macromolecule dispersing agent and polymerization inhibitor, and make it fully dissolve, mix all
Even；
(3) under agitation described precious metal salt solution is joined in step (2) in the reductant solution of gained；
(4) above-mentioned solution be stirred continuously and ensure to react and fully carry out, backward reaction system in add surface modification
Agent, is modified powder surface；
(5) after powder body centrifugation or powder natural subsidence, with deionized water and alcohol washes for several times；
(6) dry under the conditions of 50-100 DEG C, play powder dispersion, obtain average particle size distribution expensive in the high jolt ramming of 1-3 μm
Metal-powder.
High-tap density noble metal raw powder's production technology the most according to claim 1, it is characterised in that described expensive
Slaine is the one in gold chloride, silver nitrate, Palladous nitrate., dichloro two ammino palladium, chloroplatinic acid.
High-tap density noble metal raw powder's production technology the most according to claim 1, it is characterised in that described height
Dispersal agent molecule is a kind of or the most several mixture in polyvinylpyrrolidone, polyvinyl alcohol, gelatin and arabic gum.
High-tap density noble metal raw powder's production technology the most according to claim 1, it is characterised in that described resistance
Poly-agent is a kind of or the most several mixture in Colophonium, acrylic resin and polyvinyl butyral resin.
5. according to the high-tap density noble metal raw powder's production technology described in claim 1 or 3, it is characterised in that institute
State the 5-50% that weight is precious metal salt of macromolecule dispersing agent.
6. according to the high-tap density noble metal raw powder's production technology described in claim 1 or 4, it is characterised in that institute
State the 0-5% that weight is precious metal salt of polymerization inhibitor.
High-tap density noble metal raw powder's production technology the most according to claim 1, it is characterised in that described
In step (3), described reducing agent is 1: 1 with the mass ratio of precious metal salt.
High-tap density noble metal raw powder's production technology the most according to claim 1, it is characterised in that described also
Former dose is a kind of or the most several mixture of ascorbic acid, formaldehyde, sodium hypophosphite, hydrazine hydrate, sodium sulfite.
High-tap density noble metal raw powder's production technology the most according to claim 1, it is characterised in that described table
Face modifying agent is stearic acid, caproic acid, enanthic acid, octanoic acid, n-nonanoic acid, hexadecanol, lauryl mercaptan, butyl stearate, octanoic acid second
A kind of or the most several mixture of ester.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107052362A (en) * | 2017-06-15 | 2017-08-18 | 西安宏星电子浆料科技有限责任公司 | High-specific surface area ultrafine palladium powder and preparation method thereof |
| CN107186218A (en) * | 2017-04-18 | 2017-09-22 | 王芳 | A kind of preparation method of modified superfine noble metal powder |
| CN110315090A (en) * | 2019-06-14 | 2019-10-11 | 北京氦舶科技有限责任公司 | A kind of high temperature sintering type electrocondution slurry bronze and preparation method thereof |
| CN110947980A (en) * | 2019-12-24 | 2020-04-03 | 长沙新材料产业研究院有限公司 | Preparation method of micron/submicron silver powder |
| CN111925744A (en) * | 2020-07-15 | 2020-11-13 | 烟台德邦科技有限公司 | Anti-vulcanization, high-thermal-conductivity and high-temperature-resistant conductive gold adhesive |
| CN113042736A (en) * | 2021-03-09 | 2021-06-29 | 深圳市唐域信息科技有限公司 | Noble metal articles and methods of making the same |
| CN114160803A (en) * | 2021-11-17 | 2022-03-11 | 武汉船用电力推进装置研究所（中国船舶重工集团公司第七一二研究所） | High-efficiency preparation method of high-dispersity spherical gold powder |
| CN114539824A (en) * | 2022-02-23 | 2022-05-27 | 厦门紫金矿冶技术有限公司 | Gold mud pigment and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107186218A (en) * | 2017-04-18 | 2017-09-22 | 王芳 | A kind of preparation method of modified superfine noble metal powder |
| CN107186218B (en) * | 2017-04-18 | 2019-08-09 | 王芳 | A kind of preparation method of modified superfine noble metal powder |
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| CN110315090A (en) * | 2019-06-14 | 2019-10-11 | 北京氦舶科技有限责任公司 | A kind of high temperature sintering type electrocondution slurry bronze and preparation method thereof |
| CN110947980A (en) * | 2019-12-24 | 2020-04-03 | 长沙新材料产业研究院有限公司 | Preparation method of micron/submicron silver powder |
| CN111925744A (en) * | 2020-07-15 | 2020-11-13 | 烟台德邦科技有限公司 | Anti-vulcanization, high-thermal-conductivity and high-temperature-resistant conductive gold adhesive |
| CN111925744B (en) * | 2020-07-15 | 2021-12-17 | 德邦(昆山)材料有限公司 | Anti-vulcanization, high-thermal-conductivity and high-temperature-resistant conductive gold adhesive |
| CN113042736A (en) * | 2021-03-09 | 2021-06-29 | 深圳市唐域信息科技有限公司 | Noble metal articles and methods of making the same |
| CN114160803A (en) * | 2021-11-17 | 2022-03-11 | 武汉船用电力推进装置研究所（中国船舶重工集团公司第七一二研究所） | High-efficiency preparation method of high-dispersity spherical gold powder |
| CN114539824A (en) * | 2022-02-23 | 2022-05-27 | 厦门紫金矿冶技术有限公司 | Gold mud pigment and preparation method thereof |
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