CN105458285B - A kind of silver powder preparation process controlling grain size by controlling sodium hydroxide additive amount - Google Patents
A kind of silver powder preparation process controlling grain size by controlling sodium hydroxide additive amount Download PDFInfo
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- CN105458285B CN105458285B CN201510851500.0A CN201510851500A CN105458285B CN 105458285 B CN105458285 B CN 105458285B CN 201510851500 A CN201510851500 A CN 201510851500A CN 105458285 B CN105458285 B CN 105458285B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- 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 discloses a kind of silver powder preparation processes controlling grain size by controlling sodium hydroxide additive amount, include the following steps：Step S100：It takes silver nitrate crystal to prepare silver nitrate solution respectively, sodium hydroxide crystal is taken to prepare sodium hydroxide solution, grape sugar crystal is taken to prepare glucose solution；Step S200：Under stirring, the silver nitrate solution is slowly added in the sodium hydroxide solution, solution A is obtained；Step S300：Under conditions of reaction temperature is 20 30 DEG C, the glucose solution is slowly added in the solution A and is stirred continuously to complete reaction to get solution B；Step S400：The solution B is continued after stirring a period of time, is separated by solid-liquid separation, solid washing, drying is taken, obtains silver powder.Silver powder particle size distribution range prepared by the present invention is narrow, is applicable to the printing slurry of different application system, and without poisonous and harmful substance in waste liquid, silver powder size tunable, preparation process is simple.
Description
Technical field
The present invention relates to electric slurry technical fields, in particular to one kind passing through control sodium hydroxide additive amount control grain size
Silver powder preparation process.
Background technology
Solar energy is a kind of green energy resource, because its is pollution-free, inexhaustible, the advantages that is not limited by resource advantage due to it is more next
It is more valued by people, so solar cell comes into being.Solar cell is a kind of to convert solar energy into electricity
The semiconductor devices of energy, solar cell will produce electric current under conditions of illumination, and electric collecting is got up by grid line and electrode
And it transfers out.Front electrode of solar battery and grid line be all have conductive silver paste by the silk-screen printing of high-speed, high precision,
The techniques such as low temperature drying, high temperature sintering and it is manufactured.
Solar cell front side silver paste is mainly made of silver powder, glass powder, additive and four part of organic carrier.Wherein,
The performance of silver powder is particularly important.The key technical index such as conductivity and compactness after the quality of silver paste, conductive silver paste film forming
All it is to be determined by the performance of silver powder, the factors such as shape, granularity of micro-silver powder will influence the performance of silver paste, so the preparation of silver powder
It is particularly important.
But it is existing prepare in silver powder technique, generally select hydrazine hydrate, formaldehyde or sodium hypophosphite as reducing agent and nitre
Sour silver reaction, produce waste liquid in there are toxic residuas；Moreover, the grain size inconvenience tune of silver powder particles prepared by prior art
Whole, adaptability is limited, cannot be satisfied a variety of demands in market.
Invention content
The silver powder preparation process that the purpose of the present invention is to provide a kind of by controlling sodium hydroxide additive amount control grain size,
Addition sodium hydroxide simultaneously selects glucose as reducing agent, and preparing silver powder as reducing agent using the glucose of food-grade makes production
Without toxic residua in waste liquid, the additive amount by controlling sodium hydroxide can control the grain size of final silver powder particles, simple for process,
Facilitate adjustment.
The present invention is achieved through the following technical solutions：A kind of silver powder system controlling grain size by controlling sodium hydroxide additive amount
Standby technique controls the silver powder grain size of preparation by controlling sodium hydroxide additive amount, specifically includes following steps：
Step S100：It takes silver nitrate crystal to prepare silver nitrate solution respectively, takes sodium hydroxide crystal to prepare sodium hydroxide molten
Liquid takes grape sugar crystal to prepare glucose solution；
Step S200：Under stirring, the silver nitrate solution is slowly added in the sodium hydroxide solution, is obtained molten
Liquid A；
Step S300：Under conditions of reaction temperature is 20-30 DEG C, the glucose solution is slowly added to the solution
In A and it is stirred continuously to complete reaction to get solution B；
Step S400：The solution B is continued after stirring a period of time, is separated by solid-liquid separation, solid washing, drying is taken, obtains silver-colored
Powder.
Further, the mass ratio of silver nitrate crystal and sodium hydroxide crystal is 1 in the step S100:0.46-0.54；
The average grain diameter that silver powder is made in the step S400 is 0.6-2.2um.
Further, the mass ratio of the silver nitrate crystal and sodium hydroxide crystal is 1:When 0.46, average grain diameter is made
For the silver powder of 1.5-2.2um.
Further, the mass ratio of the silver nitrate crystal and sodium hydroxide crystal is 1:When 0.51, average grain diameter is made
For the silver powder of 0.9-1.5um.
Further, the mass ratio of the silver nitrate crystal and sodium hydroxide crystal is 1:When 0.54, average grain diameter is made
For the silver powder of 0.6-0.9um.
Further, the step S100 specifically includes following steps：
Step S110：Silver nitrate crystal is added into deionized water, is stirred continuously to whole dissolvings, obtains silver nitrate solution；
Step S120：Sodium hydroxide crystal is added into deionized water, is stirred continuously to whole dissolvings, it is molten to obtain sodium hydroxide
Liquid；
Step S130：Grape sugar crystal is added into hot deionized water, is stirred continuously to whole dissolvings, it is molten to obtain glucose
Liquid.
Further, the step S200 is specifically referred to：Under stirring, the silver nitrate solution is with 1500-
The flow velocity of 1700ml/min is added in the sodium hydroxide solution, continues to stir, obtains solution A.
Further, the step S300 is specifically referred to：Under stirring, the glucose solution is with 70-130ml/
The solution A is added to get solution B in the flow velocity of min.
Further, the step S400 is specifically referred to：The solution B continues stirring a period of time, and solid, solid-liquid is precipitated
After separation, solid washing, the dry silver powder to get pure drying are taken.
Further, the step S100 specifically includes following steps：
Step S110：The silver nitrate crystal of 80000g is added into 83L deionized waters, is stirred continuously to whole dissolvings, obtains
Silver nitrate solution；
Step S120：Quantitative sodium hydroxide crystal is added into 240L deionized waters, is stirred continuously to whole dissolvings, obtains
Sodium hydroxide solution；
Step S130：The grape sugar crystal of 6664g is added into 14.4L hot deionized waters, is stirred continuously to whole dissolvings,
Obtain glucose solution；
The step S200 is specifically referred to：Under stirring, the silver nitrate solution is with the stream of 1550-1650ml/min
Speed is added in the sodium hydroxide solution, continues to stir, obtains solution A；
The step S300 is specifically referred to：Under stirring, the glucose solution is with the flow velocity of 80-120ml/min
The solution A is added, and simultaneously controlling reaction temperature is 20-30 DEG C to get solution B；
The step S400 is specifically referred to：The solution B continues to stir 20-40min, and solid is precipitated, and after separation of solid and liquid, takes
Solid washing, the dry silver powder to get pure drying.
Compared with prior art, the present invention haing the following advantages and advantageous effect：
（1）A kind of silver powder preparation process controlling grain size by controlling sodium hydroxide additive amount provided by the invention, uses
Glucose produces in waste liquid without toxic residua as reducing agent, is conducive to environmental protection；
（2）A kind of silver powder preparation process controlling grain size by controlling sodium hydroxide additive amount provided by the invention, passes through
The average grain diameter of the dosage control silver powder of sodium hydroxide is controlled, silver powder particle size range is narrow, and performance is stablized；
（3）A kind of silver powder preparation process controlling grain size by controlling sodium hydroxide additive amount provided by the invention, adjustment
The mass ratio of silver nitrate crystal and sodium hydroxide can be adjusted the final grain size for preparing silver powder, easy to operate；
（4）Through actual production certification, the yield that the present invention prepares silver powder is high.
Description of the drawings
Fig. 1 is silver powder the sweeping under 10000 times that average grain diameter prepared by preparation process of the present invention is 0.6-0.9um
Retouch electromicroscopic photograph.
Fig. 2 is silver powder the sweeping under 5000 times that average grain diameter prepared by preparation process of the present invention is 0.9-1.5um
Retouch electromicroscopic photograph.
Specific implementation mode
The present invention is described in further detail with reference to embodiment, embodiments of the present invention are not limited thereto.
Embodiment 1：
A kind of silver powder preparation process controlling grain size by controlling sodium hydroxide additive amount in the present embodiment, including following step
Suddenly：
Step S100：It takes silver nitrate crystal to prepare silver nitrate solution respectively, takes sodium hydroxide crystal to prepare sodium hydroxide molten
Liquid takes grape sugar crystal to prepare glucose solution；Including step in detail below：
Step S110：The silver nitrate crystal of 80000g is added into 83L deionized waters, is stirred continuously to whole dissolvings, obtains
Silver nitrate solution；
Step S120：The sodium hydroxide crystal of 37300-42504g is added into 240L deionized waters, is stirred continuously to complete
Portion is dissolved, and obtains sodium hydroxide solution；
Step S130：The grape sugar crystal of 6664g is added into 14.4L hot deionized waters, is stirred continuously to whole dissolvings,
Obtain glucose solution；
Step S200：Under stirring, the hydroxide is added with the flow velocity of 1600ml/min in the silver nitrate solution
In sodium solution, continues to stir, obtain solution A；
Step S300：Under stirring, the solution A is added simultaneously with the flow velocity of 100ml/min in the glucose solution
Controlling reaction temperature is 20-30 DEG C to get solution B；
Step S400：The solution B continues to stir 30min, and solid is precipitated, and after separation of solid and liquid, takes solid washing, dry,
Up to pure, dry silver powder.
The average grain diameter that silver powder preparation process prepares silver powder in the present embodiment is 0.6-2.2um.
The pH value of solution A is controlled in the present invention by controlling the additive amount of sodium hydroxide, and by pH value to step S300
The influence of middle reduction reaction rate, control generate the range of silver powder particles grain size：Step S300, that is, glucose mixes simultaneously with solution A
When reaction, the pH value of mixed solution is bigger, and the reproducibility of glucose is stronger, and the rate of reduction reaction is faster, generates silver powder
The grain size of grain is smaller；Conversely, when step S300, that is, glucose is mixed and reacted with solution A, the pH value of mixed solution is smaller, grape
The reproducibility of sugar is weaker, and the rate of reduction reaction is slower, and the grain size for generating silver powder particles is bigger.
Embodiment 2：
The present embodiment advanced optimizes on the basis of embodiment 1, a kind of by controlling the control of sodium hydroxide additive amount
The silver powder preparation process of grain size, includes the following steps：
Step S100：It takes silver nitrate crystal to prepare silver nitrate solution respectively, takes sodium hydroxide crystal to prepare sodium hydroxide molten
Liquid takes grape sugar crystal to prepare glucose solution；Including step in detail below：
Step S110：The silver nitrate crystal of 80000g is added into 83L deionized waters, is stirred continuously to whole dissolvings, obtains
Silver nitrate solution；
Step S120：The sodium hydroxide crystal of 42504g is added into 240L deionized waters, is stirred continuously to whole dissolvings,
Obtain sodium hydroxide solution；
Step S130：The grape sugar crystal of 6664g is added into 14.4L hot deionized waters, is stirred continuously to whole dissolvings,
Obtain glucose solution；
Step S200：Under stirring, the hydroxide is added with the flow velocity of 1600ml/min in the silver nitrate solution
In sodium solution, continues to stir, obtain solution A；
Step S300：Under stirring, the solution A is added simultaneously with the flow velocity of 100ml/min in the glucose solution
Controlling reaction temperature is 20-30 DEG C to get solution B；
Step S400：The solution B continues to stir 30min, and solid is precipitated, and after separation of solid and liquid, takes solid washing, dry,
Up to pure, dry silver powder.
As shown in Figure 1, the average grain diameter of silver powder is 0.6-0.9um, tap density 0.8-1.6g/cm3, specific surface area is
0.7-1.4m2/g。
Embodiment 3：
The present embodiment advanced optimizes on the basis of embodiment 1, a kind of by controlling the control of sodium hydroxide additive amount
The silver powder preparation process of grain size, includes the following steps：
Step S100：It takes silver nitrate crystal to prepare silver nitrate solution respectively, takes sodium hydroxide crystal to prepare sodium hydroxide molten
Liquid takes grape sugar crystal to prepare glucose solution；Including step in detail below：
Step S110：The silver nitrate crystal of 80000g is added into 83L deionized waters, is stirred continuously to whole dissolvings, obtains
Silver nitrate solution；
Step S120：The sodium hydroxide crystal of 40572g is added into 240L deionized waters, is stirred continuously to whole dissolvings,
Obtain sodium hydroxide solution；
Step S130：The grape sugar crystal of 6664g is added into 14.4L hot deionized waters, is stirred continuously to whole dissolvings,
Obtain glucose solution；
Step S200：Under stirring, the hydroxide is added with the flow velocity of 1600ml/min in the silver nitrate solution
In sodium solution, continues to stir, obtain solution A；
Step S300：Under stirring, the solution A is added simultaneously with the flow velocity of 100ml/min in the glucose solution
Controlling reaction temperature is 20-30 DEG C to get solution B；
Step S400：The solution B continues to stir 30min, and solid is precipitated, and after separation of solid and liquid, takes solid washing, dry,
Up to pure, dry silver powder.
As shown in Fig. 2, the average grain diameter of silver powder is 0.9-1.5um, tap density 1.3-2.0g/cm3, specific surface area is
0.5-1.0m2/g。
Embodiment 4：
The present embodiment advanced optimizes on the basis of embodiment 1, a kind of by controlling the control of sodium hydroxide additive amount
The silver powder preparation process of grain size, includes the following steps：
Step S100：It takes silver nitrate crystal to prepare silver nitrate solution respectively, takes sodium hydroxide crystal to prepare sodium hydroxide molten
Liquid takes grape sugar crystal to prepare glucose solution；Including step in detail below：
Step S110：The silver nitrate crystal of 80000g is added into 83L deionized waters, is stirred continuously to whole dissolvings, obtains
Silver nitrate solution；
Step S120：The sodium hydroxide crystal of 37300g is added into 240L deionized waters, is stirred continuously to whole dissolvings,
Obtain sodium hydroxide solution；
Step S130：The grape sugar crystal of 6664g is added into 14.4L hot deionized waters, is stirred continuously to whole dissolvings,
Obtain glucose solution；
Step S200：Under stirring, the hydroxide is added with the flow velocity of 1600ml/min in the silver nitrate solution
In sodium solution, continues to stir, obtain solution A；
Step S300：Under stirring, the solution A is added simultaneously with the flow velocity of 100ml/min in the glucose solution
Controlling reaction temperature is 20-30 DEG C to get solution B；
Step S400：The solution B continues to stir 30min, and solid is precipitated, and after separation of solid and liquid, takes solid washing, dry,
Up to pure, dry silver powder.
The average grain diameter of silver powder is 1.5-2.2um, tap density 2.2-2.8g/cm3, specific surface area 0.3-0.8m2/
g。
Embodiment 5：
A kind of silver powder preparation process controlling grain size by controlling sodium hydroxide additive amount of the present embodiment, mainly passes through
Following technical proposals are realized：Include the following steps：
Step S100：It takes silver nitrate crystal to prepare silver nitrate solution respectively, takes sodium hydroxide crystal to prepare sodium hydroxide molten
Liquid takes grape sugar crystal to prepare glucose solution；
Step S200：Under stirring, the silver nitrate solution is slowly added in the sodium hydroxide solution, is obtained molten
Liquid A；
Step S300：Under conditions of reaction temperature is 20-30 DEG C, the glucose solution is slowly added to the solution
In A and it is stirred continuously to complete reaction to get solution B；
Step S400：The solution B is continued after stirring a period of time, is separated by solid-liquid separation, solid washing, drying is taken, obtains silver-colored
Powder.
Mass ratio in preparation process of the present invention by adjusting silver nitrate crystal and sodium hydroxide crystal can prepare flat
The different silver powder of equal grain size, and the silver powder average particle size range prepared is narrow, performance is extremely close.
Embodiment 6：
The present embodiment advanced optimizes on the basis of embodiment 5, a kind of by controlling the control of sodium hydroxide additive amount
The silver powder preparation process of grain size, includes the following steps：
Step S100：It takes silver nitrate crystal to prepare silver nitrate solution respectively, takes sodium hydroxide crystal to prepare sodium hydroxide molten
Liquid takes grape sugar crystal to prepare glucose solution；The step S100 specifically includes following steps：
Step S110：Silver nitrate crystal is added into deionized water, is stirred continuously to whole dissolvings, obtains silver nitrate solution；
Step S120：Sodium hydroxide crystal is added into deionized water, is stirred continuously to whole dissolvings, it is molten to obtain sodium hydroxide
Liquid；
Step S130：Grape sugar crystal is added in the hot deionized water for being 40-50 DEG C to temperature, is stirred continuously to all molten
Solution, obtains glucose solution；
Step S200：Under stirring, the hydrogen is added with the flow velocity of 1500-1700ml/min in the silver nitrate solution
In sodium hydroxide solution, continues to stir, obtain solution A；
Step S300：Under stirring, the solution is added with the flow velocity of 70-130ml/min in the glucose solution
A is to get solution B；
Step S400：The solution B continues stirring a period of time, precipitation solid, after separation of solid and liquid, takes solid washing, does
The dry silver powder to get pure drying.
Embodiment 7：
The present embodiment advanced optimizes on the basis of embodiment 5, and the technique for preparing silver powder is：It first weighs respectively certain
The silver nitrate crystal and sodium hydroxide crystal of mass ratio prepare silver nitrate solution, by the step S120 by the step S110
Sodium hydroxide solution is prepared, while weighing appropriate grape sugar crystal and preparing glucose solution by the step S130；Then institute is pressed
It states step S200 and sodium hydroxide solution is slowly added in the silver nitrate solution prepared respectively while stirring, obtain solution A；Continue by
The glucose solution of preparation is slowly added to while stirring in the solution A by the step S300, obtains solution B；Finally
Solution B is continued to stir to solid is precipitated, takes solid washing, drying, you can obtain pure, dry silver powder particles.
When the mass ratio of silver nitrate crystal and sodium hydroxide crystal is 1:When 0.46-0.54, the average grain diameter of silver powder is made
For 0.6-2.2um.Specifically, when the mass ratio of silver nitrate crystal and sodium hydroxide crystal is 1:When 0.46, the flat of silver powder is made
Equal grain size is 1.5-2.2um；When the mass ratio of silver nitrate crystal and sodium hydroxide crystal is 1:When 0.51, being averaged for silver powder is made
Grain size is 0.9-1.5um；When the mass ratio of silver nitrate crystal and sodium hydroxide crystal is 1:When 0.46, the average grain of silver powder is made
Diameter is 0.6-0.9um.
The other parts of the present embodiment are same as Example 5, and so it will not be repeated.
Embodiment 8：
A kind of silver powder preparation process controlling grain size by controlling sodium hydroxide additive amount of the present embodiment, mainly passes through
Following technical proposals are realized：Include the following steps：
Step S100：It takes silver nitrate crystal to prepare silver nitrate solution respectively, takes sodium hydroxide crystal to prepare sodium hydroxide molten
Liquid takes grape sugar crystal to prepare glucose solution.
The step S100 specifically includes following steps：
Step S110：Silver nitrate crystal is added into deionized water, is stirred continuously to whole dissolvings, obtains silver nitrate solution；
Step S120：Sodium hydroxide crystal is added into deionized water, is stirred continuously to whole dissolvings, it is molten to obtain sodium hydroxide
Liquid；
Step S130：Grape sugar crystal is added into hot deionized water, is stirred continuously to whole dissolvings, it is molten to obtain glucose
Liquid.
Step S110 is specifically referred to：The silver nitrate crystal of 80000g is added into 83L deionized waters, is stirred continuously to whole
Dissolving, obtains silver nitrate solution.
Step S120 is specifically referred to：Quantitative sodium hydroxide crystal is added into 240L deionized waters, is stirred continuously to complete
Portion is dissolved, and obtains sodium hydroxide solution.
Step S130 is specifically referred to：Into 14.4L hot deionized waters be added 6664g grape sugar crystal, be stirred continuously to
All dissolvings, obtain glucose solution.
Hot deionized water in the step S130 refers to the deionized water that temperature is 40-50 DEG C.
Step S200：Under stirring, the silver nitrate solution is slowly added in the sodium hydroxide solution, is obtained molten
Liquid A.
The step S200 is specifically referred to：Under stirring, the silver nitrate solution is with the stream of 1500-1700ml/min
Speed is added in the sodium hydroxide solution, continues to stir, obtains solution A.
Step S300：Under conditions of reaction temperature is 20-30 DEG C, the glucose solution is slowly added to the solution
In A and it is stirred continuously to complete reaction to get solution B.
The step S300 is specifically referred to：Under stirring, the glucose solution is with the flow velocity of 70-130ml/min
The solution A is added to get solution B.
Step S400：The solution B is continued after stirring a period of time, is separated by solid-liquid separation, solid washing, drying is taken, obtains silver-colored
Powder.
The step S400 is specifically referred to：The solution B continues to stir 20-40min, and solid is precipitated, and after separation of solid and liquid, takes
Solid washing, the dry silver powder to get pure drying.
The solid being precipitated in the step S400 first uses deionized water and ethyl alcohol alternately to wash, then low temperature drying.
The washing specifically includes following steps：
Step S411：First pass is carried out with deionized water to wash；
Step S412：Second time washing is carried out with ethyl alcohol；
Step S413：Third is carried out all over washing with deionized water；
Step S414：The 4th time washing is carried out with ethyl alcohol；
Step S415：The 5th time washing is carried out with deionized water；
Step S416：The 6th time washing is carried out with ethyl alcohol.
The drying specifically refer to by：Silver powder after washing is put into 60-80 DEG C of drying box, toasts 4-12h.
The drying can be carried out in vacuum drying chamber, in particular to：Silver powder after washing is put into vacuum drying chamber,
It is 0.7*10 to extract air to vacuum degree by mechanical pump-3Pa-0.9*10-3Then Pa makes baking temperature in vacuum drying chamber again
It is slowly increased to 60-80 DEG C, continues to toast 4-12h, obtains pure, dry silver powder.By the silver powder after washing, it is in vacuum degree
0.8*10-3In the environment of Pa, temperature are 70 DEG C, 6h is toasted, you can obtain pure, dry silver powder particles.
The mass ratio of the silver nitrate crystal and sodium hydroxide crystal is 1:When 0.46-0.54, obtained average grain diameter is
The silver powder of 0.6-2.2um.
The mass ratio of the silver nitrate crystal and sodium hydroxide crystal is 1:When 0.46, it is 1.5- that average grain diameter, which is made,
The silver powder of 2.2um.
The mass ratio of the silver nitrate crystal and sodium hydroxide crystal is 1:When 0.51, it is 0.9- that average grain diameter, which is made,
The silver powder of 1.5um.
The mass ratio of the silver nitrate crystal and sodium hydroxide crystal is 1:When 0.54, it is 0.6- that average grain diameter, which is made,
The silver powder of 0.9um.
Embodiment 9：
A kind of silver powder preparation process controlling grain size by controlling sodium hydroxide additive amount in the present embodiment, including following step
Suddenly：
Step S100：It is 1 to weigh mass ratio respectively:0.46-0.54:0.0833 silver nitrate solution, sodium hydroxide solution,
Glucose solution simultaneously produces corresponding solution；Specifically include following steps：
Step S110：1 part of silver nitrate crystal is added into deionized water, is stirred continuously to whole dissolvings, it is molten to obtain silver nitrate
Liquid；
Step S120：0.46-0.54 parts of sodium hydroxide crystal are added into deionized water, are stirred continuously to whole dissolvings,
Obtain sodium hydroxide solution；
Step S130：0.0833 part of grape sugar crystal is added into hot deionized water, is stirred continuously to whole dissolvings, obtains Portugal
Grape sugar juice；
Step S200：Under stirring, the hydrogen is added with the flow velocity of 1550-1650ml/min in the silver nitrate solution
In sodium hydroxide solution, continues to stir 10-40min, obtain solution A；
Step S300：Under stirring, the solution is added with the flow velocity of 80-120ml/min in the glucose solution
A is to get solution B；
Step S400：The solution B continues to stir 25-35min, and solid is precipitated, and after separation of solid and liquid, takes solid washing, dry
The dry silver powder to get pure drying.
The solid being precipitated in the step S400 first uses deionized water and ethyl alcohol alternately to wash, then low temperature drying.It is described to wash
It washs and specifically includes following steps：
Step S411：First pass is carried out with deionized water to wash；
Step S412：Second time washing is carried out with ethyl alcohol；
Step S413：Third is carried out all over washing with deionized water；
Step S414：The 4th time washing is carried out with ethyl alcohol；
Step S415：The 5th time washing is carried out with deionized water；
Step S416：The 6th time washing is carried out with ethyl alcohol.
The drying specifically refer to by：Silver powder after washing is put into 60-80 DEG C of drying box, toasts 4-12h.
Embodiment 10：
A kind of silver powder preparation process controlling grain size by controlling sodium hydroxide additive amount, includes the following steps：
Step S100：It is 1 to weigh mass ratio respectively:0.46:0.0833 silver nitrate solution, sodium hydroxide solution, grape
Sugar juice simultaneously produces corresponding solution；Specifically include following steps：
Step S110：1 part of silver nitrate crystal is added into deionized water, is stirred continuously to whole dissolvings, it is molten to obtain silver nitrate
Liquid；
Step S120：0.46 part of sodium hydroxide crystal is added into deionized water, is stirred continuously to whole dissolvings, obtains hydrogen-oxygen
Change sodium solution；
Step S130：0.0833 part of grape sugar crystal is added into hot deionized water, is stirred continuously to whole dissolvings, obtains Portugal
Grape sugar juice；
Step S200：Under stirring, the hydroxide is added with the flow velocity of 1650ml/min in the silver nitrate solution
In sodium solution, continues to stir 15min, obtain solution A；
Step S300：Under stirring, the solution A is added with the flow velocity of 120ml/min in the glucose solution, i.e.,
Obtain solution B；
Step S400：The solution B continues to stir 30min, and solid is precipitated, and after separation of solid and liquid, takes solid washing, dry,
It is 1.5-2.2um, pure, dry silver powder up to average grain diameter.
The solid being precipitated in the step S400 first uses deionized water and ethyl alcohol alternately to wash, then low temperature drying.It is described to wash
It washs and specifically includes following steps：
Step S411：First pass is carried out with deionized water to wash；
Step S412：Second time washing is carried out with ethyl alcohol；
Step S413：Third is carried out all over washing with deionized water；
Step S414：The 4th time washing is carried out with ethyl alcohol；
Step S415：The 5th time washing is carried out with deionized water；
Step S416：The 6th time washing is carried out with ethyl alcohol.
The drying specifically refer to by：Silver powder after washing is put into 65 DEG C of drying box, toasts 7h.
Embodiment 11：
A kind of silver powder preparation process controlling grain size by controlling sodium hydroxide additive amount, includes the following steps：
Step S100：It is 1 to weigh mass ratio respectively:0.51:0.0833 silver nitrate solution, sodium hydroxide solution, grape
Sugar juice simultaneously produces corresponding solution；Specifically include following steps：
Step S110：1 part of silver nitrate crystal is added into deionized water, is stirred continuously to whole dissolvings, it is molten to obtain silver nitrate
Liquid；
Step S120：0.51 part of sodium hydroxide crystal is added into deionized water, is stirred continuously to whole dissolvings, obtains hydrogen-oxygen
Change sodium solution；
Step S130：0.0833 part of grape sugar crystal is added into hot deionized water, is stirred continuously to whole dissolvings, obtains Portugal
Grape sugar juice；
Step S200：Under stirring, the hydroxide is added with the flow velocity of 1600ml/min in the silver nitrate solution
In sodium solution, continues to stir 30min, obtain solution A；
Step S300：Under stirring, the solution A is added with the flow velocity of 90ml/min in the glucose solution, i.e.,
Obtain solution B；
Step S400：The solution B continues to stir 30min, and solid is precipitated, and after separation of solid and liquid, takes solid washing, dry,
Up to pure, dry silver powder.
The solid being precipitated in the step S400 first uses deionized water and ethyl alcohol alternately to wash, then low temperature drying.It is described to wash
It washs and specifically includes following steps：
Step S411：First pass is carried out with deionized water to wash；
Step S412：Second time washing is carried out with ethyl alcohol；
Step S413：Third is carried out all over washing with deionized water；
Step S414：The 4th time washing is carried out with ethyl alcohol；
Step S415：The 5th time washing is carried out with deionized water；
Step S416：The 6th time washing is carried out with ethyl alcohol.
The drying specifically refer to by：Silver powder after washing is put into 70 DEG C of drying box, toasts 7h.
Embodiment 12：
A kind of silver powder preparation process controlling grain size by controlling sodium hydroxide additive amount, includes the following steps：
Step S100：It is 1 to weigh mass ratio respectively:0.53:0.0833 silver nitrate solution, sodium hydroxide solution, grape
Sugar juice simultaneously produces corresponding solution；Specifically include following steps：
Step S110：1 part of silver nitrate crystal is added into deionized water, is stirred continuously to whole dissolvings, it is molten to obtain silver nitrate
Liquid；
Step S120：0.53 part of sodium hydroxide crystal is added into deionized water, is stirred continuously to whole dissolvings, obtains hydrogen-oxygen
Change sodium solution；
Step S130：0.0833 part of grape sugar crystal is added into hot deionized water, is stirred continuously to whole dissolvings, obtains Portugal
Grape sugar juice；
Step S200：Under stirring, the hydroxide is added with the flow velocity of 1750ml/min in the silver nitrate solution
In sodium solution, continues to stir 30min, obtain solution A；
Step S300：Under stirring, the solution A is added with the flow velocity of 90ml/min in the glucose solution, i.e.,
Obtain solution B；
Step S400：The solution B continues to stir 30min, and solid is precipitated, and after separation of solid and liquid, takes solid washing, dry,
Up to pure, dry silver powder.
The solid being precipitated in the step S400 first uses deionized water and ethyl alcohol alternately to wash, then low temperature drying.It is described to wash
It washs and specifically includes following steps：
Step S411：First pass is carried out with deionized water to wash；
Step S412：Second time washing is carried out with ethyl alcohol；
Step S413：Third is carried out all over washing with deionized water；
Step S414：The 4th time washing is carried out with ethyl alcohol；
Step S415：The 5th time washing is carried out with deionized water；
Step S416：The 6th time washing is carried out with ethyl alcohol.
The drying specifically refer to by：Silver powder after washing is put into 65 DEG C of drying box, toasts 7h.
The above is only presently preferred embodiments of the present invention, not does limitation in any form to the present invention, it is every according to
According to the technical spirit of the present invention to any simple modification, equivalent variations made by above example, the protection of the present invention is each fallen within
Within the scope of.
Claims (9)
1. a kind of silver powder preparation process controlling grain size by controlling sodium hydroxide additive amount, it is characterised in that：By controlling hydrogen
Sodium oxide molybdena additive amount controls the silver powder grain size of preparation, specifically includes following steps：
Step S100：It takes silver nitrate crystal to prepare silver nitrate solution respectively, takes sodium hydroxide crystal to prepare sodium hydroxide solution, take
Grape sugar crystal prepares glucose solution；
Step S200：Under stirring, the silver nitrate solution is slowly added in the sodium hydroxide solution, solution A is obtained；
Step S300：Under conditions of reaction temperature is 20-30 DEG C, the glucose solution is slowly added in the solution A
And it is stirred continuously to complete reaction to get solution B；
Step S400：The solution B is continued after stirring a period of time, is separated by solid-liquid separation, solid washing, drying is taken, obtains silver powder；
The mass ratio of silver nitrate crystal and sodium hydroxide crystal is 1 in the step S100:0.46-0.54；The step S400
In be made silver powder average grain diameter be 0.6-2.2um.
2. a kind of silver powder preparation process controlling grain size by controlling sodium hydroxide additive amount according to claim 1,
It is characterized in that：The mass ratio of the silver nitrate crystal and sodium hydroxide crystal is 1:When 0.46, it is 1.5- that average grain diameter, which is made,
The silver powder of 2.2um.
3. a kind of silver powder preparation process controlling grain size by controlling sodium hydroxide additive amount according to claim 1,
It is characterized in that：The mass ratio of the silver nitrate crystal and sodium hydroxide crystal is 1:When 0.51, it is 0.9- that average grain diameter, which is made,
The silver powder of 1.5um.
4. a kind of silver powder preparation process controlling grain size by controlling sodium hydroxide additive amount according to claim 1,
It is characterized in that：The mass ratio of the silver nitrate crystal and sodium hydroxide crystal is 1:When 0.54, it is 0.6- that average grain diameter, which is made,
The silver powder of 0.9um.
5. being prepared according to a kind of silver powder controlling grain size by controlling sodium hydroxide additive amount of claim 1-4 any one of them
Technique, it is characterised in that：The step S100 specifically includes following steps：
Step S110：Silver nitrate crystal is added into deionized water, is stirred continuously to whole dissolvings, obtains silver nitrate solution；
Step S120：Sodium hydroxide crystal is added into deionized water, is stirred continuously to whole dissolvings, obtains sodium hydroxide solution；
Step S130：Grape sugar crystal is added into hot deionized water, is stirred continuously to whole dissolvings, obtains glucose solution.
6. being prepared according to a kind of silver powder controlling grain size by controlling sodium hydroxide additive amount of claim 1-4 any one of them
Technique, it is characterised in that：The step S200 is specifically referred to：Under stirring, the silver nitrate solution is with 1500-
The flow velocity of 1700ml/min is added in the sodium hydroxide solution, continues to stir, obtains solution A.
7. being prepared according to a kind of silver powder controlling grain size by controlling sodium hydroxide additive amount of claim 1-4 any one of them
Technique, it is characterised in that：The step S300 is specifically referred to：Under stirring, the glucose solution is with 70-130ml/
The solution A is added to get solution B in the flow velocity of min.
8. being prepared according to a kind of silver powder controlling grain size by controlling sodium hydroxide additive amount of claim 1-4 any one of them
Technique, it is characterised in that：The step S400 is specifically referred to：The solution B continues stirring a period of time, and solid, solid-liquid is precipitated
After separation, solid washing, the dry silver powder to get pure drying are taken.
9. being prepared according to a kind of silver powder controlling grain size by controlling sodium hydroxide additive amount of claim 1-4 any one of them
Technique, it is characterised in that：
The step S100 specifically includes following steps：
Step S110：The silver nitrate crystal of 80000g is added into 83L deionized waters, is stirred continuously to whole dissolvings, obtains nitric acid
Silver-colored solution；
Step S120：Quantitative sodium hydroxide crystal is added into 240L deionized waters, is stirred continuously to whole dissolvings, obtains hydrogen-oxygen
Change sodium solution；
Step S130：The grape sugar crystal of 6664g is added into 14.4L hot deionized waters, is stirred continuously to whole dissolvings, obtains Portugal
Grape sugar juice；
The step S200 is specifically referred to：Under stirring, the silver nitrate solution is added with the flow velocity of 1550-1650ml/min
Enter in the sodium hydroxide solution, continues to stir, obtain solution A；
The step S300 is specifically referred to：Under stirring, the glucose solution is added with the flow velocity of 80-120ml/min
The solution A and controlling reaction temperature are 20-30 DEG C to get solution B；
The step S400 is specifically referred to：The solution B continues to stir 20-40min, and solid is precipitated, and after separation of solid and liquid, takes solid
Washing, the dry silver powder to get pure drying.
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| CN101088679A (en) * | 2007-07-11 | 2007-12-19 | 中国印钞造币总公司 | Prepn process of micro silver powder |
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