CN114833334A - Method for continuously preparing micron-sized spherical gold powder - Google Patents
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- CN114833334A CN114833334A CN202210378429.9A CN202210378429A CN114833334A CN 114833334 A CN114833334 A CN 114833334A CN 202210378429 A CN202210378429 A CN 202210378429A CN 114833334 A CN114833334 A CN 114833334A
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- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
Abstract
The invention provides a method for continuously preparing micron-sized spherical gold powder with uniform particle size. The method adopts a rapid rotation nucleation method which can effectively reduce the interference of the external environment on gold particle nucleation, and comprises the steps of simultaneously introducing gold-containing mother liquor and a reducing agent into a rapid rotation nucleation reactor, rapidly completing mass transfer reaction in micro-nano liquid drops generated by high-speed rotation cutting to form a huge amount of uniform crystal nuclei, then introducing the crystal nuclei into a post-reactor, continuously completing the controllable growth of spherical gold powder crystal grains until spherical gold powder particles with micron-sized particle size range are obtained, precipitating, washing and drying the obtained micron-sized spherical gold powder, and obtaining the spherical gold powder with uniform particle size. By adopting the method, the spherical gold powder with high purity, good dispersibility, smooth surface, more uniform particle size distribution than that of the common liquid phase reduction method and average particle size D50 of 1-3 mu m can be continuously prepared.
Description
Technical Field
The invention relates to the technical field of functional materials, in particular to a method for continuously preparing micron-sized spherical gold powder for electronic paste.
Background
With the rapid development of advanced manufacturing industries such as 5G communication, radar electronics, intelligent automobiles and the like in the electronic information industry, the market demand for electronic components such as hybrid multi-chip modules (MCM-C/D), microwave hybrid integrated circuits and high-power micro-assembly chips is also increased explosively. Because gold has the conductivity second to that of silver and copper, excellent corrosion resistance and oxidation resistance, and meanwhile, gold generally has no electromigration, the gold jointly determines the inherent advantages of preparing electronic components with high frequency, low loss and long service life as a conductor functional phase of electronic paste, and the gold conductor paste also becomes an indispensable important basic material in the development direction of miniaturization, integration and high frequency of the electronic information industry.
The key performance parameters of the gold conductor slurry mainly depend on the key characteristics of the gold powder particles, such as purity, morphology, particle size distribution, specific surface area, tap density, surface property and the like, of a metal functional phase, wherein the micron-sized spherical gold powder with narrow particle size distribution is regarded as one of the key components essential for preparing the high-quality conductor gold slurry. Foreign large-scale electronic paste production enterprises such as Ferro, DuPont and Heraeus start to develop gold paste products for decades earlier than China, and mainstream manufacturers with multiple and complete gold paste products, advanced technical process and extremely high market share are developed at present. In recent years, the domestic electronic paste industry has been stricken and has come up with a lot of scientific research and production units for the research and development of gold paste products, but still is basically in the stage of imitating and running foreign products, in particular to the most critical gold powder preparation link, and the patent with the patent authorization number of CN200410090637.0 discloses a preparation method of micron-sized spherical gold powder, wherein the particle size of gold particles is 4-8 mu m, and the gold particles are suitable for decoration but not for the use of thick-film printed conductor paste; patent No. CN201610485407.7 discloses a preparation method of micron-sized flaky gold powder, but a preparation method of non-spherical gold powder. For a gold paste user, the consistency and stability of gold paste products in different batches directly determine the quality stability of downstream products, the batch stability of the gold paste products depends on the process stability of gold powder batch preparation, and a domestic research and development unit does not have a public report of a process method for preparing micron-sized spherical gold powder with narrow particle size distribution in batches due to factors such as development process or development cost, but the technical bottleneck that the domestic high-quality gold paste needs to break through in the industrialization process is solved.
Disclosure of Invention
The invention aims to provide a method for preparing micron-sized spherical gold powder for electronic paste in batches.
In order to solve the technical problem, the invention provides a method for preparing micron-sized spherical gold powder for electronic paste in batches, which comprises the following steps:
firstly, preparing a gold fulminate suspension A;
step two, preparing ascorbic acid and dispersant solution B;
thirdly, mixing the suspension A and the solution B for nucleation to obtain a reaction solution C;
and step four, depositing, washing, centrifuging and drying.
The first step is to prepare gold-containing mother liquor with certain concentration and volume into a gold fulminate suspension A and regulate and control the pH value of the suspension A.
Adding a proper amount of organic dispersant into an organic reducing agent with certain concentration and volume, and uniformly stirring to form a solution B;
and the third step is to pump the suspension A and the solution B into a fast rotary nucleation reactor simultaneously by adopting a fast rotary nucleation method to fast rotate and react to form reaction liquid C which is collected and continuously led out from the side wall of the reactor.
Wherein the fourth step is to introduce the reaction solution C into multiple groups of gold-containing mother liquor with the same concentration and temperature Liquid reactor D 1 、D 2 、D 3 、...、D n (n is more than or equal to 1 natural number), continuously heating at constant temperature and stirring with strong current to grow crystal nucleus to form gold powder precipitate, stopping heating and stirring after a certain time, pouring out each group of gold powder precipitate by decantation, combining the precipitates, washing by deionized boiling water until no chloride ion is detected, adding absolute ethyl alcohol for washing, centrifuging, and drying in vacuum to obtain micron-sized spherical gold powder with uniform particle size.
Wherein the first step is to use HAuCl with the mass concentration of Au of 20-30 g/L 4 Adding dilute ammonia water with the concentration of 5-8 wt% into the aqueous solution to form a gold fulminate suspension A.
In the first step, ammonia water is used for regulating and controlling the pH value of the suspension A to be 3.5-4.0.
Wherein, the organic reducing agent in the second step is ascorbic acid, and the organic dispersant is polyvinyl alcohol.
Wherein, the mass ratio of Au to VC to PVA is 5 to 10 (1-1.2).
Wherein the third step further rotation rate is 2500-3000 rpm.
The invention also provides micron-sized spherical gold powder prepared by the method, wherein the gold powder has an average particle size D 50 ＝1～3μm。
The invention has the advantages of
The preparation method of the gold powder can be used for industrial stable mass production of micron-sized spherical gold powder. Because the grain nucleation and growth processes of the gold powder are carried out separately, the difference between batches after the mass production of the gold powder is smaller than that of the common liquid phase reduction method, theoretically, as long as the raw material preparation is sufficient, and the volume, the quantity and the conditions of the subsequent reaction container D are controlled in place, the micron-sized spherical gold powder (with the production capacity of more than or equal to 10 kg/batch) with narrow particle size distribution and various target yields can be continuously and continuously produced in a single batch, and the preparation of the gold powder with larger yield is realized by continuously expanding the volume of the reaction container and regulating and searching new process parameters unlike the common liquid phase reduction method.
The method can continuously prepare the spherical gold powder with high purity, good dispersibility, smooth surface, more uniform particle size distribution than that of the common liquid phase reduction method and average particle size D50 of 1-3 mu m.
Drawings
FIG. 1 is a scanning electron microscope for observing the morphology of the gold powder prepared in example 1.
Detailed Description
By adopting the method provided by the invention, uniform crystal nuclei of gold powder particles can be continuously and uninterruptedly generated and led out in a rapid rotary nuclear reactor with small volume (15-20L), the generated crystal nuclei are led out to a parallel container for gold particle growth according to the target yield of the gold powder, and as long as the raw material preparation is sufficient and the number and conditions of subsequent reaction containers are controlled in place, the method can be used for uninterruptedly and continuously producing micron-sized spherical gold powder with narrow particle size distribution (with the production capacity of more than or equal to 10 kg/batch), thereby providing a brand-new and reliable technical method and a technological route for industrial mass production of micron-sized spherical gold powder with narrow particle size distribution.
The method of the invention can continuously prepare the average grain diameter D with high purity, good dispersibility, smooth surface, more uniform grain diameter distribution than the common liquid phase reduction method 50 The gold powder is 1-3 mu m spherical gold powder, and can be used for preparing thick film gold paste for electronic components such as mixed multi-chip modules (MCM-C/D), microwave mixed integrated circuits, high-power micro-assembly chips and the like.
The invention provides a method for preparing micron-sized spherical gold powder for electronic paste in batches, which comprises the following steps:
firstly, preparing a gold fulminate suspension A;
step two, preparing ascorbic acid and dispersant solution B;
thirdly, mixing the suspension A and the solution B for nucleation to obtain a reaction solution C;
and step four, depositing, washing, centrifuging and drying.
The first step is to further specifically prepare HAuCl with the mass concentration of Au of 20-30 g/L 4 Adding dilute ammonia water with the concentration of 5-8 wt% into an aqueous solution (the impurity content is less than or equal to 0.005 wt%) to form a gold fulminate suspension A, and regulating the pH of the suspension A to be 3.5-4.0 by using the ammonia water.
The second step is to mix an ascorbic acid (VC) aqueous solution with a mass concentration of 100g/L and a polyvinyl alcohol (PVA, molecular weight of 25000-35000) aqueous solution with a concentration of 2-5 wt% and stir the mixture uniformly to form a solution B, wherein the mass ratio of Au to VC to PVA is 5:10 (1-1.2).
And the third step is further specifically that a rapid rotation nucleation method is adopted, the suspension A and the solution B are simultaneously pumped into a rapid rotation nucleation reactor to rapidly rotate (the rotation rate is 2500-3000 rpm) and perform reaction nucleation, and a reaction solution C is continuously formed on the side wall of the rapid rotation nucleation reactor with the volume of 15-20L and collected and led out.
The fourth step is to introduce the reaction liquid C into n (n is more than or equal to 1 natural number) reaction liquid with similar volume and HAuCl with same concentration and temperature 4 A plurality of groups of reactors D for aqueous solution (Au mass concentration is 20-50 g/L; solution temperature is 20-70 ℃, and impurity content is less than or equal to 0.005wt percent) 1 、D 2 、D 3 、...、D n Continuously heating at constant temperature and stirring with strong current for 1-2 hours to grow crystal nucleus to form gold powder precipitate, after stopping heating and stirring for 0.5-1 hours, pouring out all groups of gold powder precipitate by a decantation method, combining the precipitates, washing by deionized boiling water until no chloride ion is detected, then adding absolute ethyl alcohol for washing, centrifuging and drying in vacuum to obtain micron-sized spherical gold powder with uniform particle size.
Embodiments of the present invention will be described in detail below with reference to examples and drawings, by which how to apply technical means to solve technical problems and achieve a technical effect can be fully understood and implemented.
Then 3 groups of reactors are rapidly rotated at different rotating speeds to prepare gold grain crystal nuclei under different raw material concentration ratios, and different quantities of gold-containing mother liquor are subsequently adopted to carry out gold grain growth so as to obtain single batch of spherical gold powder with different quantities.
Example 1
A commercially available chloroauric acid aqueous solution (the impurity content is less than or equal to 0.005 wt%) is used as a raw material (the gold can also be prepared by a nitrate removal method after pure gold is dissolved by adding aqua regia), and a gold trichloride solution with the mass concentration of 20g/L of Au is prepared by using a 500mL volumetric flask for later use. Pouring the prepared gold trichloride solution into a beaker, stirring at room temperature, and dropwise adding about 70mL of 5% diluted ammonia water to form a gold fulminate suspension A with the pH value of 3.5 for later use.
According to the mass ratio of Au to VC to PVA of 5 to 10 to 1, 1L of VC aqueous solution with the mass concentration of 100g/L is prepared by 20gVC, and the VC aqueous solution is poured into a 2L beaker containing 500g of PVA aqueous solution with the concentration of 2 wt% to be mixed and stirred at room temperature to form uniform liquid B for later use.
Adopting a rapid rotational nucleation method, simultaneously spraying A and B into a rapid rotational nucleation reactor with a volume of about 18L by using a peristaltic pump (the pumping flow rate of the pump A is 2mL/s, the pumping flow rate of the pump B is 5.3mL/s), adjusting the rotating speed of a rotating packed bed to 3000rpm for reaction nucleation, continuously collecting a reaction solution C flowing out of a lower port of the rapid rotational nucleation reactor, introducing the reaction solution C into HAuCl containing 20g/L of Au in mass concentration and at a temperature of 70 DEG C 4 Continuously heating at a constant temperature of 70 ℃ and stirring with strong current for 1 hour in a reactor D (the volume of the reactor is 5L) with 2L of aqueous solution to grow crystal nuclei to form gold powder precipitate, stopping heating and stirring for 1 hour, pouring out the gold powder precipitate in the reactor D by a decantation method, washing the precipitate by deionized boiling water until no chloride ion is detected, adding absolute ethyl alcohol for washing for 3 times, and carrying out rapid centrifugation and vacuum drying at 60 ℃ to obtain 48.6g of gold powder. Inspection of average particle diameter D of gold powder by laser particle sizer 50 The gold powder is observed to be spherical under a scanning electron microscope, and the particle size of the gold powder is approximately distributed in the range of 0.8-3.2 μm, as shown in figure 1.
50g of spherical gold powder was prepared in a single batch.
Example 2
A commercially available chloroauric acid aqueous solution (the impurity content is less than or equal to 0.005 wt%) is used as a raw material (the gold can also be prepared by a nitrate removal method after pure gold is dissolved by adding aqua regia), and a gold trichloride solution with the mass concentration of Au of 25g/L is prepared by using a 1L volumetric flask for later use. Pouring the prepared gold trichloride solution into a beaker, and dropwise adding about 130mL of 8% ammonia water at room temperature while stirring to form a gold fulminate suspension A with the pH of 3.7 for later use.
According to the mass ratio of Au to VC to PVA of 5:10:1.1, 200gVC is used for preparing 2L of VC aqueous solution with the mass concentration of 100g/L, and the VC aqueous solution is poured into a 5L beaker containing 440g of PVA aqueous solution with the concentration of 5 wt% to be mixed and stirred at room temperature to form uniform liquid B for later use.
Adopting a rapid rotational nucleation method, simultaneously spraying A and B into a rapid rotational nucleation reactor with the volume of about 18L by using peristaltic pumps (the pumping flow rate of the pump A is 2mL/s, the pumping flow rate of the pump B is 4.3mL/s), adjusting the rotation rate of a rotating packed bed to 2800rpm for reaction nucleation, continuously collecting a reaction solution C flowing out of a lower port of the rapid rotational nucleation reactor, timing from the beginning of the reaction solution C flowing out of the rapid rotational nucleation reactor to 283s, and introducing the C into HAuCl containing 37.5g/L of Au in mass concentration and the temperature of 60 DEG C 4 Continuously heating at constant temperature of 60 ℃ and stirring under strong flow for 1.5 hours in a reactor D1 (the volume of the reactor is 5L) containing 1L of aqueous solution to grow crystal nuclei and form gold powder precipitate; the reaction solution C was discharged for 283s, and HAuCl containing Au at a mass concentration of 37.5g/L and a temperature of 60 ℃ was introduced into the whole of the remaining portion 4 Continuously heating at constant temperature of 60 ℃ and stirring under strong flow for 1.5 hours in a reactor D2 (the volume of the reactor is 5L) containing 1L of aqueous solution to grow crystal nuclei and form gold powder precipitate; errors of solution temperature and concentration in D1 and D2 are less than or equal to +/-2%, after reactant precipitates stop heating and stirring for 45min, the gold powder precipitates in the combined reactors D1 and D2 are poured out by a decantation method, the precipitates are washed by deionized boiling water until no chloride ion is detected, then absolute ethyl alcohol is added for washing for 3 times, and the gold powder 96.3g is obtained by quick centrifugation and vacuum drying at 60 ℃. Method for detecting average grain diameter D of gold powder by using laser particle sizer 50 The gold powder is observed to be spherical under a scanning electron microscope, and the particle size of the gold powder is approximately distributed in the range of 0.7-4.0 mu m.
100g of spherical gold powder was prepared in a single batch.
Example 3
A commercially available chloroauric acid aqueous solution (the impurity content is less than or equal to 0.005 wt%) is used as a raw material (the gold can also be prepared by a nitrate removal method after pure gold is dissolved by adding aqua regia), and a gold trichloride solution with the mass concentration of 30g/L of Au is prepared by using a 1L volumetric flask for later use. Pouring the prepared gold trichloride solution into a beaker, stirring at room temperature, and dropwise adding about 200mL of 6% ammonia water to form a gold fulminate suspension A with the pH value of 4.0 for later use.
Preparing 3L of VC aqueous solution with the mass concentration of 100g/L by 300gVC according to the mass ratio of Au to VC to PVA of 5:10:1.2, pouring the VC aqueous solution into a 5L beaker containing 720g of PVA aqueous solution with the concentration of 5 wt%, and mixing and stirring at room temperature to form uniform liquid B for later use.
Adopting a rapid rotary nucleation method, simultaneously spraying A and B into a rapid rotary nucleation reactor with the volume of about 18L by using peristaltic pumps (the pumping flow rate of the pump A is 1.5mL/s, the pumping flow rate of the pump B is 4.7mL/s), adjusting the rotation speed of a rotary packed bed to 2500rpm for reaction nucleation, continuously collecting a reaction liquid C flowing out of a lower port of the rapid rotary nucleation reactor, starting timing from the outflow of the reaction liquid C from the rapid rotary nucleation reactor to 267s, and introducing the C into HAuCl containing 50g/L of Au in mass concentration and at the temperature of 25 DEG C 4 In a reactor D1 (the volume of the reactor is 5L) with 800mL of aqueous solution, continuously heating at the constant temperature of 25 ℃ and stirring with strong current for 2 hours to grow crystal nuclei and form gold powder precipitate; the reaction solution C flowed out 267s to 533s and HAuCl containing Au at a mass concentration of 50g/L and a temperature of 25 ℃ was introduced 4 In a reactor D2 (the volume of the reactor is 5L) with 800mL of aqueous solution, continuously heating at the constant temperature of 25 ℃ and stirring with strong current for 2 hours to grow crystal nuclei and form gold powder precipitate; after the reaction solution C flowed out for 533 seconds, HAuCl containing Au at a mass concentration of 50g/L and a temperature of 25 ℃ was introduced into the whole of the remaining portion 4 In a reactor D3 (the volume of the reactor is 5L) with 800mL of aqueous solution, continuously heating at the constant temperature of 25 ℃ and stirring with strong current for 2 hours to grow crystal nuclei and form gold powder precipitate; errors of the solution temperature and concentration in D1, D2 and D3 are less than or equal to +/-2%, after the reactant precipitates in D1, D2 and D3 are stopped heating and stirred for 30min, the gold powder precipitates in the combined reactors D1, D2 and D3 are poured out by a decantation method, the precipitates are washed by deionized boiling water until no chloride ion is detected, then absolute ethyl alcohol is added for washing for 3 times, and the gold powder 140.7g is obtained by quick centrifugation and vacuum drying at 60 ℃. Method for detecting average grain diameter D of gold powder by using laser particle sizer 50 The gold powder is observed to be spherical under a scanning electron microscope, and the particle size of the gold powder is approximately distributed between 1.0 and 4.3 mu m.
150g of spherical gold powder was prepared in a single batch.
All of the above mentioned intellectual property rights are not intended to be restrictive to other forms of implementing the new and/or new products. Those skilled in the art will take advantage of this important information, and the foregoing will be modified to achieve similar performance. However, all modifications or alterations are based on the new products of the invention and belong to the reserved rights.
The foregoing is directed to preferred embodiments of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow. However, any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention are within the protection scope of the technical solution of the present invention.
Claims (10)
1. A method for preparing micron-sized spherical gold powder for electronic paste in batch is characterized by comprising the following steps:
firstly, preparing a gold fulminate suspension A;
step two, preparing ascorbic acid and dispersant solution B;
thirdly, mixing the suspension A and the solution B for nucleation to obtain a reaction solution C;
and step four, depositing, washing, centrifuging and drying.
2. The method according to claim 1, wherein the micron-sized spherical gold powder for electronic paste mass production comprises: the first step is to prepare gold-containing mother liquor with certain concentration and volume into a gold fulminate suspension A and regulate and control the pH value of the suspension A.
3. The method according to claim 1, wherein the micron-sized spherical gold powder for electronic paste mass production comprises: and the second step is further to specifically add an organic reducing agent with certain concentration and volume into a proper amount of organic dispersing agent and uniformly stir the mixture to form a solution B.
4. The method according to claim 1, wherein the micron-sized spherical gold powder for electronic paste mass production comprises: and the third step is to pump the suspension A and the solution B into a fast rotary nucleation reactor simultaneously by adopting a fast rotary nucleation method to fast rotate and react to form reaction liquid C which is collected from the side wall of the reactor and continuously led out.
5. The method according to claim 1, wherein the micron-sized spherical gold powder for electronic paste mass production comprises: the fourth step is to introduce the reaction solution C into a plurality of groups of reactors D containing mother liquor containing gold with the same concentration and temperature 1 、D 2 、D 3 、...、D n (n is more than or equal to 1 natural number), continuously heating at constant temperature and stirring with strong current to grow crystal nucleus to form gold powder precipitate, stopping heating and stirring after a certain time, pouring out each group of gold powder precipitate by decantation, combining the precipitates, washing by deionized boiling water until no chloride ion is detected, adding absolute ethyl alcohol for washing, centrifuging, and drying in vacuum to obtain micron-sized spherical gold powder with uniform particle size.
6. The method according to claim 2, wherein the micron-sized spherical gold powder for electronic paste mass production comprises: the first step is to further specifically prepare HAuCl with the mass concentration of Au of 20-30 g/L 4 Adding dilute ammonia water with the concentration of 5-8 wt% into the aqueous solution to form a gold fulminate suspension A.
7. The method according to claim 6, wherein the micron-sized spherical gold powder for electronic paste mass production comprises: and in the first step, ammonia water is used for regulating and controlling the pH value of the suspension A to be 3.5-4.0.
8. The method according to claim 6, wherein the micron-sized spherical gold powder for electronic paste mass production comprises: in the second step, the organic reducing agent is ascorbic acid, and the organic dispersing agent is polyvinyl alcohol.
9. The method for mass production of micron-sized spherical gold powder for electronic paste according to claim 3, wherein: and the mass ratio of Au to VC to PVA is 5 to 10 (1-1.2).
10. Use of any of claims 1 to 9The micron-sized spherical gold powder prepared by the method has the average grain diameter D 50 ＝1～3μm。
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| WO2010066335A1 (en) * | 2008-12-12 | 2010-06-17 | Byk-Chemie Gmbh | Method for producing metal nanoparticles and nanoparticles obtained in this way and use thereof |
| CN102245333A (en) * | 2008-12-12 | 2011-11-16 | 比克化学股份有限公司 | Method for producing metal nanoparticles and nanoparticles obtained in this way and use thereof |
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