CN114833334B - Method for continuously preparing micron-sized spherical gold powder - Google Patents
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- CN114833334B CN114833334B CN202210378429.9A CN202210378429A CN114833334B CN 114833334 B CN114833334 B CN 114833334B CN 202210378429 A CN202210378429 A CN 202210378429A CN 114833334 B CN114833334 B CN 114833334B
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F9/00—Making metallic powder or suspensions thereof
- 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 'fast rotation nucleation method' capable of effectively reducing the interference of external environment on gold particle nucleation, simultaneously introduces gold-containing mother liquor and a reducing agent into a fast rotation nucleation reactor, rapidly completes mass transfer reaction in micro-nano liquid drops generated by high-speed rotation cutting to form huge amount of uniform crystal nuclei, then introduces the crystal nuclei into a post-reactor, continuously completes the controllable growth of spherical gold powder crystal grains until obtaining the spherical gold powder particles with the micron-sized particle size range, and then deposits, washes and dries the obtained micron-sized spherical gold powder to obtain the spherical gold powder with uniform particle size. The method can continuously prepare the spherical gold powder with high purity, good dispersibility, smooth surface, more uniform particle size distribution than the common liquid phase reduction method, and average particle size D50=1-3 mu m.
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, and intelligent automobiles 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-assembled chips has also exploded. Gold has conductivity inferior to silver and copper, excellent corrosion resistance and oxidation resistance, and meanwhile, gold generally has no electromigration, so that the points together determine the inherent advantages of gold as a conductor functional phase of electronic paste for preparing high-frequency, low-loss and long-service-life electronic components, and the gold conductor paste also becomes an important basic material indispensable for 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 metal functional phase, namely the purity, morphology, particle size distribution, specific surface area, tap density, surface property and the like of gold powder particles, wherein micron-sized spherical gold powder with narrow particle size distribution is regarded as one of the key components necessary for preparing high-quality conductor gold slurry. The overseas large-scale electronic paste manufacturers such as Ferro, duPont, heraeus start to develop gold paste products in decades earlier than domestic, and the gold paste products are currently developed into main stream manufacturers with various and complete types, advanced technical process and extremely high market share. In recent years, the domestic electronic paste industry has been in the spotlight and has emerged a batch of scientific research and production units for developing gold paste products, but is still basically in the stage of imitating and following foreign products, especially in the most critical gold powder preparation link, the patent with patent grant number CN200410090637.0 discloses a preparation method of micron-sized spherical gold powder, the particle size of the gold particles is 4-8 mu m, and the gold powder is suitable for decoration rather than thick film printing conductor paste application; patent No. CN201610485407.7 discloses a preparation method of micron-sized flake gold powder, but a preparation method of non-spherical gold powder. For gold slurry users, the consistency and stability of gold slurry products among different batches directly determine the quality stability of downstream products, the batch stability of gold slurry products depends on the process stability of gold powder batch preparation, and the domestic research and development units have not yet reported a process method for batch preparation of micron-sized spherical gold powder with narrow particle size distribution because of factors such as development progress or development cost, which is a technical bottleneck that must be broken through in the industrialization of domestic high-quality gold slurry.
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 problems, the invention provides a method for preparing micron-sized spherical gold powder for electronic paste in batches, which comprises the following steps:
firstly, preparing gold-rapamycin suspension A;
secondly, preparing an ascorbic acid and dispersant solution B;
thirdly, mixing the suspension A and the solution B for nucleation to obtain a reaction solution C;
and fourthly, depositing, washing, centrifuging and drying.
The first step is to prepare gold-containing mother solution with a certain concentration and volume into gold-bearing suspension A, and regulate the pH value of the suspension A.
Wherein, the second step is to add a proper amount of organic dispersant into an organic reducer with a certain concentration and volume and stir the mixture uniformly to form a solution B;
the third step is to pump the suspension A and the solution B into a fast rotation nucleation reactor for fast rotation and reaction nucleation simultaneously by adopting a fast rotation nucleation method, so that the reaction liquid C is collected from the side wall of the reactor and is continuously led out.
Wherein the fourth step is to introduce the reaction liquid C into a plurality of groups of reactors D containing gold-containing mother liquid with the same concentration and temperature 1 、D 2 、D 3 、...、D n And (n is more than or equal to 1 natural number), continuously heating at constant temperature and stirring with strong flow to enable crystal nucleus to grow up to form gold powder precipitates, stopping heating and stirring after a certain time, pouring out each group of gold powder precipitates by using a decantation method, merging the precipitates, washing with deionized boiling water until no chloride ions are detected, then adding absolute ethyl alcohol for washing, centrifuging and vacuum drying to obtain micron-sized spherical gold powder with uniform particle size.
Wherein the first step is more specifically to make the mass concentration of Au be 20-30 g/L HAuCl 4 Adding dilute ammonia water with the concentration of 5-8wt% into the aqueous solution to form gold-ralate suspension A.
Wherein, in the first step, ammonia water is used for regulating and controlling the PH=3.5-4.0 of the suspension A.
Wherein the organic reducing agent in the second step is ascorbic acid, and the organic dispersing agent is polyvinyl alcohol.
Wherein in the second step, the mass ratio of the three components is Au to VC, PVA=5:10 (1-1.2).
Wherein the third step further rotates at a speed of 2500-3000 rpm.
The invention also provides micron-sized spherical gold powder prepared by the method, wherein the gold powder has an average particle diameter D 50 ＝1～3μm。
The beneficial effects of the invention are that
The preparation method of the gold powder can be used for industrialized stable mass production of micron-sized spherical gold powder. As the nucleation and growth processes of gold powder crystal grains are carried out separately, the batch-to-batch difference of the gold powder after the mass production is smaller than that of the common liquid phase reduction method, theoretically, as long as the raw materials are prepared fully and the volume, the quantity and the conditions of a subsequent reaction container D are controlled in place, micron-sized spherical gold powder (with the production capacity of more than or equal to 10 kg/batch) with narrow particle size distribution of various target yields in a single batch can be continuously produced without interruption, and the preparation of gold powder with larger yield is realized by continuously expanding the volume of the reaction container and regulating and controlling new technological parameters unlike the common liquid phase reduction method.
The invention can continuously prepare the spherical gold powder with high purity, good dispersibility, smooth surface, more uniform particle size distribution than the common liquid phase reduction method and average particle size D50=1-3 mu m.
Drawings
FIG. 1 is a view of the morphology of the gold powder prepared in example 1 under a scanning electron microscope.
Detailed Description
The method provided by the invention can continuously generate and export uniform crystal nuclei of gold powder particles in a rapid rotary nucleation reactor with small volume (15-20L), and continuously export the generated crystal nuclei into parallel containers for gold particle growth according to the target yield of gold powder, and the method provided by the invention can continuously produce micron-sized spherical gold powder with narrow particle size distribution (with the production capacity of more than or equal to 10 kg/batch) as long as the raw materials are prepared fully and the number and conditions of subsequent reaction containers are controlled in place, thereby providing a novel and reliable technical method and process route for industrially producing micron-sized spherical gold powder with narrow particle size distribution.
By usingThe method of the invention can continuously prepare the catalyst with high purity, good dispersibility, smooth surface, more uniform particle size distribution and average particle size D compared with the common liquid phase reduction method 50 Spherical gold powder of 1-3 μm, which 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-assembled 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 gold-rapamycin suspension A;
secondly, preparing an ascorbic acid and dispersant solution B;
thirdly, mixing the suspension A and the solution B for nucleation to obtain a reaction solution C;
and fourthly, depositing, washing, centrifuging and drying.
The first step is further specifically to make the mass concentration of Au be 20-30 g/L HAuCl 4 Adding dilute ammonia water with the concentration of 5-8wt% into the aqueous solution (the impurity content is less than or equal to 0.005 wt%) to form gold-thunder suspension A, and regulating the PH=3.5-4.0 of the suspension A by using the ammonia water.
The second step is to prepare an ascorbic acid (VC) aqueous solution with the mass concentration of 100g/L and a polyvinyl alcohol (PVA) aqueous solution with the concentration of 2-5 wt% according to the mass ratio of Au to VC to PVA=5 to 10 (1-1.2), and uniformly stirring the mixture to form a solution B.
The third step is to pump the suspension A and the solution B into a fast rotation nucleation reactor simultaneously by adopting a fast rotation nucleation method (the rotation speed is 2500-3000 rpm) to perform fast rotation and perform reaction nucleation, and continuously form a reaction solution C on the side wall of the fast rotation nucleation reactor with the volume of 15-20L and collect and guide out the reaction solution C.
The fourth step is to introduce the reaction liquid C into n (n is greater than or equal to 1 natural number) with similar volumes and hold HAuCl with the same concentration and temperature 4 Multiple groups of reactors D for aqueous solution (Au mass concentration 20-50 g/L; solution temperature 20-70 ℃ and impurity content less than or equal to 0.005 wt%) 1 、D 2 、D 3 、...、D n In the middle, constantly at a constant levelHeating and stirring for 1-2 hr to grow crystal nucleus to form gold powder precipitate, stopping heating and stirring for 0.5-1 hr, decanting to separate gold powder precipitate, merging the precipitate, washing with deionized boiling water to no chlorine ion, washing with absolute alcohol, centrifuging and vacuum drying to obtain micron level spherical gold powder with homogeneous particle size.
The following examples and drawings are used to describe embodiments of the present invention in detail, thereby solving the technical problems by applying the technical means to the present invention, and realizing the technical effects can be fully understood and implemented accordingly.
The method comprises the steps of preparing gold grain crystal nuclei by using 3 groups of fast rotating nucleation reactors at different raw material concentration ratios and different rotation speeds, and subsequently adopting different amounts of gold-containing mother liquor to perform gold grain growth so as to obtain single-batch spherical gold powder with different amounts.
Example 1
The commercial chloroauric acid aqueous solution (the impurity content is less than or equal to 0.005 wt%) is taken as a raw material (the solution can be prepared by adding pure gold into aqua regia for dissolution and then adopting a nitrate removal method), and a 500mL volumetric flask is used for preparing the gold trichloride solution with the Au mass concentration of 20g/L for standby. The prepared gold trichloride solution was poured into a beaker and stirred at room temperature dropwise with about 70mL of 5% strength dilute aqueous ammonia to form gold-Lei-ate suspension a having ph=3.5 for use.
According to the mass ratio of Au to VC to PVA=5:10:1, 20g gVC is used for preparing 1L of VC aqueous solution with the mass concentration of 100g/L, and the VC aqueous solution is poured into a 2L beaker containing 500g of PVA aqueous solution with the concentration of 2wt% to be mixed and stirred at room temperature to form uniform liquid B for standby.
Adopting a rapid rotary nucleation method, spraying A and B into a rapid rotary nucleation reactor with a volume of about 18L simultaneously by a peristaltic pump (A pump flow rate=2 mL/s, B pump flow rate=5.3 mL/s), regulating the rotation rate of a rotary packed bed to 3000rpm for reaction nucleation, continuously collecting a reaction solution C flowing out of the lower opening of the rapid rotary nucleation reactor, and introducing the reaction solution C into HAuCl with Au mass concentration of 20g/L and temperature of 70 DEG C 4 In a reactor D (the volume of the reactor is 5L) with 2L of aqueous solution, heating at a constant temperature of 70 ℃ and stirring with strong current for 1 hour continuously to enable crystal nuclei to grow to form gold powder precipitate, and stopping heating and stirringAfter 1 hour, the gold powder precipitate in the reactor D was decanted, washed with deionized boiling water until no chloride ions were detected, washed 3 times with absolute ethanol, and dried under vacuum at 60℃by rapid centrifugation to obtain 48.6g of gold powder. Testing the average grain diameter D of gold powder by a laser particle size analyzer 50 The morphology of the gold powder was observed under a scanning electron microscope to be spherical, and the particle size of the gold powder was observed to be approximately 0.8 to 3.2 μm, as shown in fig. 1.
50g of spherical gold powder was prepared in a single batch.
Example 2
The commercial chloroauric acid aqueous solution (the impurity content is less than or equal to 0.005 wt%) is taken as a raw material (the solution can be prepared by adding pure gold into aqua regia for dissolution and then adopting a nitrate removal method), and a 1L volumetric flask is used for preparing the gold trichloride solution with the Au mass concentration of 25g/L for later use. The prepared gold trichloride solution was poured into a beaker and stirred at room temperature dropwise with about 130mL of 8% strength aqueous ammonia to form gold-Lei-ate suspension a having ph=3.7 for use.
According to the mass ratio of Au to VC to PVA=5:10:1.1, preparing 2L of VC aqueous solution with the mass concentration of 100g/L by using 200gVC, pouring the VC aqueous solution into a 5L beaker containing 440g of PVA aqueous solution with the mass concentration of 5wt% and mixing and stirring at room temperature to form uniform liquid B for standby.
Adopting a rapid rotary nucleation method, spraying A and B into a rapid rotary nucleation reactor with a volume of about 18L by a peristaltic pump (A pump flow rate=2 mL/s, B pump flow rate=4.3 mL/s), regulating the rotation rate of a rotary packed bed to 2800rpm for reaction nucleation, continuously collecting a reaction solution C flowing out of the lower opening of the rapid rotary nucleation reactor, and introducing C into HAuCl with an Au mass concentration of 37.5g/L and a temperature of 60 ℃ from the reaction solution C from the beginning of the outflow of the rapid rotary nucleation reactor to 283s 4 In a reactor D1 (the volume of the reactor is 5L) with 1L of aqueous solution, heating at a constant temperature of 60 ℃ and stirring for 1.5 hours under strong current to enable crystal nuclei to grow to form gold powder precipitates; introducing the whole of the remainder of the effluent 283s of the reaction solution C into HAuCl having a mass concentration of 37.5g/L of Au and a temperature of 60 ℃ 4 In a reactor D2 (the volume of the reactor is 5L) with 1L of aqueous solution, heating at a constant temperature of 60 ℃ and stirring for 1.5 hours under strong current to enable crystal nuclei to grow to form gold powder precipitates; errors in the temperature and concentration of solutions in D1 and D2And after the reactant precipitation is stopped from heating and stirring for 45min, pouring out the gold powder precipitates in the combined reactors D1 and D2 by a decantation method, washing the precipitates by deionized boiling water until no chloride ions are detected, adding absolute ethyl alcohol for washing for 3 times, and obtaining 96.3g of gold powder by quick centrifugation and vacuum drying at 60 ℃. Testing the average grain diameter D of gold powder by a laser particle size analyzer 50 The morphology of the gold powder is observed to be spherical under a scanning electron microscope, and the particle size of the gold powder is observed to be approximately distributed between 0.7 and 4.0 μm.
100g of spherical gold powder was prepared in a single batch.
Example 3
The commercial chloroauric acid aqueous solution (the impurity content is less than or equal to 0.005 wt%) is taken as a raw material (the solution can be prepared by adding pure gold into aqua regia for dissolution and then adopting a nitrate removal method), and a 1L volumetric flask is used for preparing the gold trichloride solution with the Au mass concentration of 30g/L for standby. The prepared gold trichloride solution was poured into a beaker and stirred at room temperature dropwise with about 200mL of aqueous ammonia having a concentration of 6% to form gold-Lei-ate suspension a having ph=4.0 for use.
According to the mass ratio of Au to VC to PVA=5:10:1.2, 300gVC is used for preparing 3L of VC water solution with the mass concentration of 100g/L, and the VC water solution is poured into a 5L beaker containing 720g of PVA water solution with the mass concentration of 5wt% to be mixed and stirred at room temperature to form uniform liquid B for standby.
Adopting a rapid rotary nucleation method, spraying A and B into a rapid rotary nucleation reactor with a volume of about 18L by a peristaltic pump (A pump flow rate=1.5 mL/s, B pump flow rate=4.7 mL/s), regulating the rotation rate of a rotary packed bed to 2500rpm for reaction nucleation, continuously collecting a reaction solution C flowing out of the lower opening of the rapid rotary nucleation reactor, and introducing C into HAuCl with Au mass concentration of 50g/L and temperature of 25 ℃ from the beginning of the reaction solution C flowing out of the rapid rotary nucleation reactor to 267s 4 In a reactor D1 (the volume of the reactor is 5L) with 800mL of aqueous solution, heating at constant temperature of 25 ℃ and stirring with strong current for 2 hours continuously to enable crystal nuclei to grow to form gold powder sediment; the whole of the portion of the reaction liquid C from 267s to 533s was introduced with HAuCl having a mass concentration of 50g/L of Au and a temperature of 25 ℃ 4 In a reactor D2 (the volume of the reactor is 5L) with 800mL of aqueous solution, heating is continuously carried out at the constant temperature of 25 ℃ and stirring is carried out for 2 hours under strong current to enable crystal nuclei to grow up to form gold powder sedimentPrecipitating; after 533s of the reaction solution C was discharged, the whole of the remaining portion was introduced with HAuCl having a mass concentration of 50g/L of Au and a temperature of 25 ℃ 4 In a reactor D3 (the volume of the reactor is 5L) with 800mL of aqueous solution, heating at constant temperature of 25 ℃ and stirring with strong current for 2 hours continuously to enable crystal nuclei to grow to form gold powder sediment; and D1, D2 and D3, after the reactant precipitates in D1, D2 and D3 are stopped heating and stirring for 30min, pouring out the gold powder precipitates in the combined reactors D1, D2 and D3 by a decantation method, washing the precipitates by deionized boiling water until no chloride ions are detected, adding absolute ethyl alcohol for washing for 3 times, and carrying out rapid centrifugation and vacuum drying at 60 ℃ to obtain 140.7g of gold powder. Testing the average grain diameter D of gold powder by a laser particle size analyzer 50 The morphology of the gold powder is observed to be spherical under a scanning electron microscope, and the particle size of the gold powder is observed to be approximately distributed between 1.0 and 4.3 μm.
150g of spherical gold powder was prepared in a single batch.
All of the above-described primary implementations of this intellectual property are not intended to limit other forms of implementing this new product and/or new method. Those skilled in the art will utilize this important information and the above modifications to achieve a similar implementation. However, all modifications or adaptations belong to the reserved rights based on the new products of the invention.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the invention in any way, and any person skilled in the art may make modifications or alterations to the disclosed technical content to the equivalent embodiments. However, any simple modification, equivalent variation and variation of the above embodiments according to the technical substance of the present invention still fall within the protection scope of the technical solution of the present invention.
Claims (5)
1. A method for batch preparation of micron-sized spherical gold powder for electronic paste, comprising the steps of:
firstly, preparing gold-rapamycin suspension A;
secondly, preparing an ascorbic acid and dispersant solution B;
thirdly, pumping the suspension A and the solution B into a rapid rotation nucleation reactor simultaneously by a rapid rotation nucleation method to rapidly rotate and react for nucleation, and collecting and continuously guiding out a reaction solution C from the side wall of the reactor;
fourth, the reaction solution C is led into a plurality of groups of reactors D containing gold-containing mother solution with the same concentration and temperature 1 、D 2 、D 3 、...、D n Wherein n is more than or equal to 1 natural number, heating at constant temperature and stirring with strong flow continuously to enable crystal nucleus to grow up to form gold powder precipitate, stopping heating and stirring after 1-2 hours, pouring out each group of gold powder precipitate by decantation, merging the precipitate, washing with deionized boiling water until no chloride ions are detected, then adding absolute ethyl alcohol for washing, centrifuging and vacuum drying, thus obtaining micron-sized spherical gold powder with uniform particle size.
2. The method for mass production of micron-sized spherical gold powder for electronic paste according to claim 1, wherein: the first step is further specifically to make the mass concentration of Au be 20-30 g/L HAuCl 4 Adding dilute ammonia water with the concentration of 5-8wt% into the aqueous solution to form gold-ralate suspension A.
3. The method for mass production of micron-sized spherical gold powder for electronic paste according to claim 1, wherein: the second step is to prepare an ascorbic acid (VC) aqueous solution with the mass concentration of 100g/L, mix the ascorbic acid (VC) aqueous solution with the concentration of 2-5wt% and stir the mixture uniformly to form a solution B.
4. The method for mass-producing micron-sized spherical gold powder for electronic paste according to claim 2, wherein: in the first step, ammonia water is used for regulating and controlling the PH=3.5-4.0 of the suspension A.
5. The micron-sized spherical gold powder prepared by the method of any one of claims 1 to 4, wherein the gold powder has an average particle diameter D 50 ＝1～3μm。
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| CN104289728A (en) * | 2014-10-23 | 2015-01-21 | 苏州华冲精密机械有限公司 | Preparation method of spherical superfine gold powder for electronic materials |
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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 |
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