CN104910652B - A kind of bronze movable type pigment and preparation method thereof - Google Patents
A kind of bronze movable type pigment and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of bronze movable type pigment, comprise the following steps：(1) electrolytic copper powder and zinc powder are weighed, two kinds of materials are mixed with batch mixer；(2) material for being well mixed step (1), which is sent into, carries out High temperature diffusion heat treatment in sintering furnace；(3) material for being heat-treated step (2) High temperature diffusion carries out ultra-fine grinding after primary solution is broken with ultrafine crusher；(4) material of step (3) ultra-fine grinding is subjected to mechanical alloying milled processed with high energy ball mill, obtains the bronze movable type pigment.The bronze movable type pigment of the present invention is that the mode being combined using High temperature diffusion, ultra-fine grinding, three kinds of technologies of mechanical alloy is produced by the use of electrolytic copper powder and zinc powder as raw material, and its simple production process, product particle size are small, coating effect is good.
Description
Technical field
The invention belongs to metallic powdery pigment field, and in particular to a kind of bronze movable type pigment and preparation method thereof.
Background technology
Metallic pigments are a kind of Special Categories in coatings industry, originating from being chased after in auto industry to metallic luster outward appearance
Ask, and be a kind of coating accepted and applied extensively by consumer.With the development of modern society, with metal light
Application of the product of damp outward appearance in plant equipment, electronic product and automobile external decoration is more and more extensive, and this decoration effect
The coating of fruit starts gradually to penetrate into the various aspects of people's life.Now, by light-coloured coating and the eye-catching gold of visual effect
Category coating is combined to obtain the visual effect of uniqueness.Therefore, industry to the demand of metallic paint, species also increasingly
Greatly, relatively common metallic pigments have aluminium powder, zinc powder, copper base metal powder etc., and all these metallic pigments are by metal or conjunction
Gold composition, is characterized in form and aspect and gloss with metal.
With the improvement of people ' s living standards with the progress of esthetic sentiment, consumer proposes higher requirement to product,
Especially in today of market competition increasingly fierceness, not only require that product has the interior quality of function admirable, and require it
Product appearance or outer packing is exquisite, high-end, air, improve grade.Gold production signifies rich and noble, is used as expensive goods
Application or packing and decorating, have played great sales promotion function.Such as currently a popular so-called " local tyrant's gold " just illustrates this point, domestic
The outward appearance of all popular metal effect with gold color of outer automobile, electronic product, therefore bronze movable type pigment is wide
The general decoration for being applied to high-grade goods or automobile, and market can be increasing.
In addition, developing rapidly with electronics industry, Electromagnetic Interference turns into the killer of human health, meanwhile, electromagnetism
Wave interference can also cause electronic equipment unstable, cause information leakage, jeopardize national interests and safety.Bronze movable type is applied
Material is the characteristics of Cu-Zn alloy powder has low surface resistivity and high anti-oxidation, is widely used cheap material, is well suited as leading
The conductive base-material of electrocoating paint, its composition is copper-zinc (Cu-Zn) alloyed powder, there is different models and form and aspect, Zn by Zn content differences
Electrode potential is lower than Cu, because cathodic protection effect can protect Cu not oxidized well, it is possible to utilize Cu-Zn alloy powder coating
And coating is made into, serve the efficiency of electromagnetic shielding.
Copper base metal pigment-Cu-Zn alloy powder (hereinafter referred to as Cu-Zn alloy powder) is to pass through one kind that certain process is made by copper, zinc
A kind of flake metal powder with imitative golden effect.Most of high-grade bronze movable type pigment that the country is used is that foreign countries enter
Mouthful, its particle size is small, function admirable, price high.It is by certain first by copper, zinc that the Cu-Zn alloy powder mode of production traditional at present, which is,
Ratio carry out melting, after the copper alloy of fusing dusts through atomization, be put into after ball mill grinding in wet bulb grinding machine, wet-milling are crushed through moving back
Fire, dry and refined in the smart ball mill of feeding, the powder after fine grinding after classification, trapping, polishing product.Traditional country is raw
The technology for producing bronze movable type pigment falls behind than external, and its metal pigment particle size is larger, production cost is high.
The content of the invention
In view of the shortcomings of the prior art, an object of the present invention is to provide a kind of preparation of bronze movable type pigment
Method, its simple production process, product particle size are small, coating effect is good.
For up to this purpose, the present invention uses following technical scheme：
A kind of preparation method of bronze movable type pigment, comprises the following steps：
(1) electrolytic copper powder and zinc powder are weighed, two kinds of materials are mixed with batch mixer；
(2) material for being well mixed step (1), which is sent into, carries out High temperature diffusion heat treatment in sintering furnace；
(3) material for being heat-treated step (2) High temperature diffusion carries out superfine powder after primary solution is broken with ultrafine crusher
It is broken；
(4) material of step (3) ultra-fine grinding is subjected to mechanical alloying milled processed with high energy ball mill, obtains institute
State bronze movable type pigment.
Wherein, batch mixer is one kind of double helix stirring and Double cone mixer in step (1).
The High temperature diffusion technology of step (2)：The electrolytic copper powder of well mixed different proportion and the mixture of zinc powder according to
Certain weight, feed rate, be passed through between being sent to 550~800 DEG C reproducibility or protective atmosphere (but also vacuum shape
State) under sintering furnace in carry out the High temperature diffusion heat treatment regular hour so that fusing point melts for 419.53 DEG C of zinc powder
Melt liquid phase and diffuse in the electrolytic copper powder particle that also non-liquid phase occurs, because electrolytic copper powder appearance is shaped as the tree of irregular
Dendritic, its powder granule has flourishing hole, hole and surface area, so fusing, the Zn-ef ficiency of liquid phase can be easy to be expanded
Dissipate or be absorbed to inside electrolytic copper powder particle and formed certain copper-kirsite mutually even alloy structure and Zn-ef ficiency diffusion,
It is evenly distributed.Spread due to Zn-ef ficiency, distribution it is uniform, so material after the High temperature diffusion is heat treated also has face
The yellow of the uniform ormolu of color, gold lustre.In addition, the High temperature diffusion technology of the electrolytic copper powder and zinc powder can also pass through
Electrolytic copper powder and the ratio of zinc powder, the temperature and time of High temperature diffusion is adjusted to adjust alloy color and the gloss under different requirements
Brightness.
Wherein, reducing atmosphere and one kind of protective atmosphere are passed through in the sintering furnace in step (2), or sintering furnace is true
Dummy status.Reducing atmosphere can be hydrogen, and protective atmosphere can be neutral gas such as nitrogen, inert gas such as argon gas or a variety of
The mixed gas of gas such as carbon monoxide, carbon dioxide, hydrogen, methane, the nitrogen of gas mixing composition.
Wherein, the High temperature diffusion heat treatment temperature in step (2) be 550~800 DEG C, such as 550 DEG C, 600 DEG C, 650 DEG C,
700 DEG C, 750 DEG C, 800 DEG C, High temperature diffusion heat treatment time is 0.5~3h, such as 0.5h, 1h, 1.5h, 2h, 2.5h, 3h.
The superfine technique of step (3)：Dendroid, particle inner void, hole are shaped as using electrolytic copper powder appearance
Flourishing, apparent density is low, thus it can be caused to sinter that neck is fragile, consistency is low after High temperature diffusion is heat-treated, material combine compared with
Loosely, the characteristic of low intensity, recycles the ultrafine crusher that machinery and air-flow crushing are combined to expand the copper zinc after High temperature diffusion
Dissipate alloyed powder and carry out physical crushing.Because the fusing point of zinc is 419.53 DEG C, and proportion is fewer than copper, so after High temperature diffusion
Zn-ef ficiency can all melt, diffuse into electrolytic copper powder, and the particle of electrolytic copper powder be in dendroid, its individual particle be all by
More small particle adhesion, with reference to being constituted, so during ultra-fine grinding is carried out, single electrolytic copper powder particle can also
Further solution is broken into more tiny copper particle.So, the ormolu material after High temperature diffusion is heat-treated is by super
Ormolu particle of the grain diameter size below 10 microns can be processed to after finely divided.
The Mechanic Alloying Technology of step (4)：Mechanical alloying refers to metal or alloy powder in high energy ball mill
By fierce Ground shock waves, collision for a long time between powder particle and abrading-ball, powder particle is iteratively produced cold welding, fracture, cause
Atoms permeating in powder particle, so as to obtain a kind of powder technology of preparing of alloying powder.In the present invention, mainly in tool
Ormolu particle is further refined using the mode of mechanical alloy in the environment of protective atmosphere, and make copper and zinc deposit
Further alloying, is electrolytic copper powder and zinc powder additionally, due to material, ductility and glossiness are all relatively good, so passing through machine
It is less than 2 microns that ormolu material, which will turn into grain size, after tool alloy treatment, and the squama with Gold production metallic luster
Sheet of copper Zinc alloy powder pigment.
Wherein, the ratio of grinding media to material of step (4) is 10~30:1, such as 10:1、15:1、20:1、25:1、30:1, abrading-ball size
For 3~10mm, such as 3mm, 4mm, 5mm, 6mm, 7mm, 8mm, 9mm, 10mm；The mechanical alloying milled processed time is 1~5h,
Such as 1h, 1.5h, 2h, 2.5h, 3h, 3.5h, 4h, 4.5h, 5h.
The color of Cu-Zn alloy powder is determined by the color of alloy, and with the difference of institute's cupric zinc ratio, Cu-Zn alloy powder is presented
Different form and aspect, can be divided into three kinds of green light, blue or green feux rouges and feux rouges：Referred to as green light Cu-Zn alloy powder of the cupric 75~80% or so,
It is green gold coloured gold powder；Be referred to as blue or green feux rouges Cu-Zn alloy powder of the cupric 84~86% or so, also known as light gold bronze, in proof gold color
Phase；Referred to as feux rouges Cu-Zn alloy powder of the cupric 88% or so, also known as pure gold bronze, in red golden phase.
Cu-Zn alloy powder particle is in sclay texture, is observed under ESEM, and the scale of Cu-Zn alloy powder is in irregular shape, and edge is in
Zigzag, the radius-thickness ratio of powder granule is typically greater than 100, and what is had can even reach 150, and Cu-Zn alloy powder requires that particle diameter distribution has
Narrow scope as far as possible.
The topmost reason why Cu-Zn alloy powder can show high gloss in binder is exactly Cu-Zn alloy powder piece tool
There is the characteristic floated in binder, metallic pigments are to assign improving flotation property to greatest extent as main performance indications.
It is because it has special surface chemistry, Cu-Zn alloy powder that Cu-Zn alloy powder accounts for one seat in packages printing industry
Glossiness turn into one of important indicator of product quality, the raising of glossiness is for improving the quality of product, with important meaning
Justice.The glossiness of metallic flake pigment depends on the size and arrangement direction of scale, when Cu-Zn alloy powder pigment and ground are in parallel
During row, with very high reflectivity, it is more neat that Cu-Zn alloy powder is aligned, and mirrored effect is more notable, and bronze printing glossiness is higher.
The second object of the present invention is to provide a kind of bronze movable type pigment, wherein, bronze movable type pigment is pressed
Mass percent meter, includes 70%~95% electrolytic copper powder, such as 70%, 75%, 78%, 80%, 82%, 85%, 87%,
90%th, 93%, 95%；5%~30% zinc powder, such as 5%, 8%, 10%, 13%, 15%, 17%, 20%, 22%,
25%th, 30%.
Wherein, electrolytic copper powder mesh number is more than 200 mesh such as 200 mesh, 250 mesh, 300 mesh, 350 mesh, 400 mesh, 500 mesh；
Zinc powder mesh number is more than 300 mesh such as 300 mesh, 350 mesh, 400 mesh, 450 mesh, 500 mesh, 600 mesh.
Compared with prior art, beneficial effects of the present invention are：A kind of preparation method of bronze movable type pigment, bag
Include following steps：(1) electrolytic copper powder and zinc powder are weighed, two kinds of materials are mixed with batch mixer；(2) step (1) is well mixed
High temperature diffusion heat treatment is carried out in material feeding sintering furnace；(3) material for being heat-treated step (2) High temperature diffusion is solved by primary
After broken ultra-fine grinding is carried out with ultrafine crusher；(4) material of step (3) ultra-fine grinding is subjected to mechanical conjunction with high energy ball mill
Aurification milled processed, obtains the bronze movable type pigment.
The bronze movable type pigment of the present invention is, by the use of electrolytic copper powder and zinc powder as raw material, to mix equal with batch mixer
But reproducibility or protective atmosphere are passed through between 550~800 DEG C are sent to after even, is carried out also in the sintering furnace under vacuum state
High temperature diffusion is heat-treated the regular hour, and the zinc powder for making fusing point be 419.53 DEG C is uniformly spread to flourishing hole, hole
Inside the dendritic electrolytic copper powder particle of gap and surface area, so the material after the High temperature diffusion is heat treated also has
The yellow of the uniform ormolu of color, gold lustre；Ormolu material sintering neck after High temperature diffusion is heat-treated is crisp
Weak, consistency is low, material combine loosely, low intensity, using machinery and the ultrafine crusher that is combined of air-flow crushing to high temperature
Copper zinc diffusion alloy powder after diffusion carries out physical crushing, makes its grain diameter size below 10 microns；With protectiveness
Ormolu particle is set further to refine using the mode of mechanical alloy in the environment of atmosphere, the copper zinc after mechanical alloy is handled
It is less than 2 microns that alloy material, which will turn into grain size, and the flakey ormolu powder with Gold production metallic luster
Pigment.The bronze movable type pigment of the present invention is, by the use of electrolytic copper powder and zinc powder as raw material, to use High temperature diffusion, ultra-fine
Crush, the mode that three kinds of technologies of mechanical alloy are combined is produced, its simple production process, product particle size are small, coating effect
It is good.
Embodiment
Technical scheme is further illustrated below by embodiment.
Unless specific instructions, various raw materials of the invention are commercially available buys, or is prepared according to the conventional method of this area
Obtain.
Embodiment 1
By mass percentage, the electrolytic copper powder of 75%250 mesh and the zinc powder of 25%400 mesh are weighed, is stirred with double helix
Batch mixer is sufficiently mixed two kinds of materials；Then, well mixed material feeding is connected with the sintering furnace of vacuum carry out it is 800 DEG C high
Warm diffusion heat treatments 1h；The material being heat-treated through High temperature diffusion is combined after primary solution is broken with machinery and air-flow crushing
Ultrafine crusher carries out ultra-fine grinding；Finally the material through ultra-fine grinding is carried out at mechanical alloying grinding with high energy ball mill
3h is managed, wherein ratio of grinding media to material is 30:1, abrading-ball is 10mm, obtains the bronze movable type pigment, tests bronze movable type face
The particle diameter and water surface covering force of material, experimental result are shown in Table 1.
Embodiment 2
By mass percentage, the electrolytic copper powder of 80%300 mesh and the zinc powder of 20%400 mesh are weighed, Double cone mixer is used
It is sufficiently mixed two kinds of materials；Then, well mixed material feeding is connected with 750 DEG C of High temperature diffusions of progress in the sintering furnace of nitrogen
It is heat-treated 1.5h；By the material being heat-treated through High temperature diffusion be combined after primary solution is broken with machinery and air-flow crushing it is ultra-fine
Pulverizer carries out ultra-fine grinding；The material through ultra-fine grinding is finally subjected to mechanical alloying milled processed with high energy ball mill
4h, wherein ratio of grinding media to material are 20:1, abrading-ball is 8mm, obtains the bronze movable type pigment, test bronze movable type pigment
Particle diameter and water surface covering force, experimental result are shown in Table 1.
Embodiment 3
By mass percentage, the electrolytic copper powder of 85%300 mesh and the zinc powder of 15%400 mesh are weighed, Double cone mixer is used
It is sufficiently mixed two kinds of materials；Then, well mixed material feeding is connected with 700 DEG C of High temperature diffusions of progress in the sintering furnace of nitrogen
It is heat-treated 1.5h；By the material being heat-treated through High temperature diffusion be combined after primary solution is broken with machinery and air-flow crushing it is ultra-fine
Pulverizer carries out ultra-fine grinding；The material through ultra-fine grinding is finally subjected to mechanical alloying milled processed with high energy ball mill
4h, wherein ratio of grinding media to material 20:1, abrading-ball is 6mm, obtains the bronze movable type pigment, tests the grain of bronze movable type pigment
Footpath and water surface covering force, experimental result are shown in Table 1.
Embodiment 4
By mass percentage, the electrolytic copper powder of 90%300 mesh and the zinc powder of 10%400 mesh are weighed, Double cone mixer is used
It is sufficiently mixed two kinds of materials；Then, well mixed material feeding is connected with 600 DEG C of High temperature diffusions of progress in the sintering furnace of nitrogen
It is heat-treated 2h；The superfine powder that the material being heat-treated through High temperature diffusion is combined after primary solution is broken with machinery and air-flow crushing
Broken machine carries out ultra-fine grinding；The material through ultra-fine grinding is finally subjected to mechanical alloying milled processed 4h with high energy ball mill,
Wherein ratio of grinding media to material 10:1, abrading-ball is 5mm, obtains the bronze movable type pigment, tests the particle diameter of bronze movable type pigment
And water surface covering force, experimental result is shown in Table 1.
Embodiment 5
By mass percentage, the electrolytic copper powder of 95%300 mesh and the zinc powder of 5%400 mesh are weighed, is filled with Double cone mixer
It is divided to mixing two kinds of materials；Then, well mixed material feeding is connected with 550 DEG C of High temperature diffusion heat of progress in the sintering furnace of nitrogen
Handle 3h；The ultra-fine grinding that the material being heat-treated through High temperature diffusion is combined after primary solution is broken with machinery and air-flow crushing
Machine carries out ultra-fine grinding；The material through ultra-fine grinding is finally subjected to mechanical alloying milled processed 4h with high energy ball mill, its
Middle ratio of grinding media to material 5:1, abrading-ball is 3mm, obtains the bronze movable type pigment, tests the particle diameter and water of bronze movable type pigment
Face covering power, experimental result is shown in Table 1.
Comparative example
By mass percentage, weigh 80% copper powder and 20% zinc powder carries out melting, the copper alloy of fusing dusts through atomization
Afterwards, ball mill grinding in horizontal high-energy stirring ball mill machine is put into, ratio of grinding media to material is 10:1, crush the powder after 2.5h and pass through sieve classification,
Bronze movable type pigment is prepared by traditional mode, the particle diameter and water surface covering force of bronze movable type pigment is tested, it is real
Test and the results are shown in Table 1.
Table 1
| Embodiment | Cu-Zn alloy powder color | Cu-Zn alloy powder particle diameter (μm) | Water surface covering force (cm2/g) |
| Embodiment 1 | Gold production | 1.6 | 9850 |
| Embodiment 2 | Bluish yellow color | 1.6 | 8924 |
| Embodiment 3 | Green lake | 1.7 | 10035 |
| Embodiment 4 | Red gold | 1.8 | 9523 |
| Embodiment 5 | Aubergine | 1.9 | 10050 |
| Comparative example | It is blue or green golden | 12.5 | 6854 |
As can be seen from Table 1, the bronze movable type pigment particle size that the present invention is prepared is below 2 microns, than tradition
The particle diameter of Cu-Zn alloy powder prepared by pattern is small；The bronze movable type pigment water surface covering force that the present invention is prepared compares traditional mode
The water surface covering force of the Cu-Zn alloy powder of preparation is big, and coating effect is more preferable.
Above example is only used for illustrating the method detailed of the present invention, the invention is not limited in above-mentioned method detailed, i.e.,
Do not mean that the present invention has to rely on above-mentioned method detailed and could implemented.Person of ordinary skill in the field is it will be clearly understood that right
Any improvement of the present invention, addition, the selection of concrete mode of equivalence replacement and auxiliary element to each raw material of product of the present invention
Deng within the scope of all falling within protection scope of the present invention and being open.
Claims (3)
1. a kind of preparation method of bronze movable type pigment, it is characterised in that comprise the following steps：
(1) electrolytic copper powder and zinc powder are weighed, two kinds of materials are mixed with batch mixer；
(2) material for being well mixed step (1), which is sent into, carries out High temperature diffusion heat treatment in sintering furnace；
(3) material for being heat-treated step (2) High temperature diffusion carries out ultra-fine grinding after primary solution is broken with ultrafine crusher；
(4) material of step (3) ultra-fine grinding is subjected to mechanical alloying milled processed with high energy ball mill, obtains described copper-based
Metallic powdery pigment；
Wherein, the High temperature diffusion heat treatment temperature in the step (2) is 550~800 DEG C, and High temperature diffusion heat treatment time is
0.5~3h；
Ultrafine crusher in the step (3) is the ultrafine crusher that mechanical crushing and air-flow crushing are combined；The step
(3) particle size of the bronze movable type pigment after ultra-fine pulverizer disintegrating is less than 10 μm；
The step (4) is specially, by the material Jing Guo step (3) ultra-fine grinding to less than 10 μm, using high energy ball mill, to adjust
Ratio of grinding media to material and abrading-ball size are saved, mechanical alloying milled processed is carried out, obtains the bronze movable type pigment；
Ratio of grinding media to material is 10~30 in the step (4):1, abrading-ball size is 3~10mm, during the mechanical alloying milled processed
Between be 1~5h；
The particle size of bronze movable type pigment after step (4) the mechanical alloying milled processed is less than 2 μm.
2. a kind of preparation method of bronze movable type pigment according to claim 1, it is characterised in that the step
(1) batch mixer is one kind of double helix stirring and Double cone mixer in.
3. a kind of preparation method of bronze movable type pigment according to claim 1, it is characterised in that the step
(2) reducing atmosphere and one kind of protective atmosphere are passed through in the sintering furnace in, or sintering furnace is vacuum state.
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| CN105542537A (en) * | 2016-03-08 | 2016-05-04 | 陈夏风 | Pigment with natural tone and stability and preparation method of pigment |
| CN106216659A (en) * | 2016-08-31 | 2016-12-14 | 昆山德泰新材料科技有限公司 | A kind of tin bronze alloys powder and preparation method thereof |
| CN108436073A (en) * | 2018-03-07 | 2018-08-24 | 金川集团股份有限公司 | A kind of production method of low-apparent-density brass powder |
| CN109135508A (en) * | 2018-08-15 | 2019-01-04 | 厦门德立邦新材料科技有限公司 | One kind imitating gold-plated powdery paints and preparation method thereof |
| CN114147229A (en) * | 2021-11-23 | 2022-03-08 | 江苏萌达新材料科技有限公司 | Preparation method of copper-zinc alloy diffusion powder |
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