CN105458285A - Silver powder preparing technology for controlling grain size through control over adding amount of sodium hydroxide - Google Patents
Silver powder preparing technology for controlling grain size through control over adding amount of sodium hydroxide Download PDFInfo
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- CN105458285A CN105458285A CN201510851500.0A CN201510851500A CN105458285A CN 105458285 A CN105458285 A CN 105458285A CN 201510851500 A CN201510851500 A CN 201510851500A CN 105458285 A CN105458285 A CN 105458285A
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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 silver powder preparing technology for controlling the grain size through control over the adding amount of sodium hydroxide. The technology comprises the following steps that S100, silver nitrate crystals are taken to prepare a silver nitrate solution, sodium hydroxide crystals are taken to prepare a sodium hydroxide solution, and glucose crystals are taken to prepare a glucose solution; S200, in the stirring state, the silver nitrate solution is slowly added in the sodium hydroxide solution, and a solution A is obtained; S300, under the condition that the reaction temperature is 20-30 DEG C, the glucose solution is slowly added into the solution A and constantly stirred till the reaction is thorough, and a solution B is obtained; and S400, the solution B continues to be stirred for a period of time, then solid and liquid separation is carried out, a solid body is taken, washed and dried, and silver powder is obtained. The prepared silver powder is small in grain size distribution range and can be suitable for printing sizing agents of different application systems, toxic and harmful substances do not exist in waste liquid, the grain size of the silver powder can be controlled, and the preparing technology is simple.
Description
Technical field
The present invention relates to electric slurry technical field, specifically referring to a kind of silver powder preparation technology controlling particle diameter by controlling NaOH addition.
Background technology
Solar energy is a kind of green energy resource, is more and more subject to people's attention, so solar cell has arisen at the historic moment because it is pollution-free, inexhaustible, not by advantages such as resource advantage restrictions.Solar cell is a kind of semiconductor devices that solar energy can be converted to electric energy, and under the condition of illumination, solar cell can generation current, to be got up by electric collecting and transfer out by grid line and electrode.Front electrode of solar battery and grid line all have conductive silver paste to be made by the technique such as serigraphy, low temperature drying, high temperature sintering of high-speed, high precision.
Solar cell front side silver paste mainly contain silver powder, glass dust, additive and organic carrier four part composition.Wherein, the performance of silver powder is particularly important.The key technical index such as the conductance after the quality of silver paste, conductive silver paste film forming and compactness are all determined by the performance of silver powder, and the factor such as shape, granularity of micro-silver powder will the performance of impact silver slurry, so the preparation of silver powder seems particularly important.
But existingly prepare in silver powder technique, usually select hydrazine hydrate, formaldehyde or sodium hypophosphite to react as reducing agent and silver nitrate, produce in waste liquid and there is toxic residua; And the particle diameter of silver powder particles prepared by existing technique is inconvenient to adjust, and adaptability is limited, the multiple demand in market cannot be met.
Summary of the invention
The object of the present invention is to provide a kind of silver powder preparation technology controlling particle diameter by controlling NaOH addition, add NaOH and select glucose as reducing agent, adopt the glucose of food-grade to prepare silver powder as reducing agent to make in production waste liquid without toxic residua, the particle diameter of final silver powder particles can be controlled, simple, the convenient adjustment of technique by the addition controlling NaOH.
The present invention is achieved through the following technical solutions: a kind of silver powder preparation technology controlling particle diameter by controlling NaOH addition, controlling, specifically comprising the following steps by controlling the silver powder particle diameter of NaOH addition to preparation:
Step S100: get silver nitrate crystal respectively and prepare liquor argenti nitratis ophthalmicus, gets NaOH crystal preparation sodium hydroxide solution, gets glucose crystal preparation glucose solution;
Step S200: under stirring, slowly adds described liquor argenti nitratis ophthalmicus in described sodium hydroxide solution, obtains solution A;
Step S300: be under the condition of 20-30 DEG C in reaction temperature, slowly adds described glucose solution in described solution A and is also constantly stirred to complete reaction, obtain solution B;
Step S400: after described solution B is continued to stir a period of time, Separation of Solid and Liquid, gets solids wash, drying, obtain silver powder.
Further, in described step S100, the mass ratio of silver nitrate crystal and NaOH crystal is 1:0.46-0.54; In described step S400, the average grain diameter of obtained silver powder is 0.6-2.2um.
Further, when the mass ratio of described silver nitrate crystal and NaOH crystal is 1:0.46, obtained average grain diameter is the silver powder of 1.5-2.2um.
Further, when the mass ratio of described silver nitrate crystal and NaOH crystal is 1:0.51, obtained average grain diameter is the silver powder of 0.9-1.5um.
Further, when the mass ratio of described silver nitrate crystal and NaOH crystal is 1:0.54, obtained average grain diameter is the silver powder of 0.6-0.9um.
Further, described step S100 specifically comprises the following steps:
Step S110: add silver nitrate crystal in deionized water, is constantly stirred to whole dissolving, obtains liquor argenti nitratis ophthalmicus;
Step S120: add NaOH crystal in deionized water, is constantly stirred to whole dissolving, obtains sodium hydroxide solution;
Step S130: add glucose crystal in hot deionized water, is constantly stirred to whole dissolving, obtains glucose solution.
Further, described step S200 specifically refers to: under stirring, and described liquor argenti nitratis ophthalmicus adds in described sodium hydroxide solution with the flow velocity of 1500-1700ml/min, continues to stir, and obtains solution A.
Further, described step S300 specifically refers to: under stirring, and described glucose solution adds described solution A with the flow velocity of 70-130ml/min, obtains solution B.
Further, described step S400 specifically refers to: described solution B continues to stir a period of time, separates out solid, after Separation of Solid and Liquid, gets solids wash, drying, obtain pure, dry silver powder.
Further, described step S100 specifically comprises the following steps:
Step S110: the silver nitrate crystal adding 80000g in 83L deionized water, is constantly stirred to whole dissolving, obtains liquor argenti nitratis ophthalmicus;
Step S120: add quantitative NaOH crystal in 240L deionized water, be constantly stirred to whole dissolving, obtain sodium hydroxide solution;
Step S130: the glucose crystal adding 6664g in 14.4L hot deionized water, is constantly stirred to whole dissolving, obtains glucose solution;
Described step S200 specifically refers to: under stirring, and described liquor argenti nitratis ophthalmicus adds in described sodium hydroxide solution with the flow velocity of 1550-1650ml/min, continues to stir, and obtains solution A;
Described step S300 specifically refers to: under stirring, and described glucose solution adds described solution A with the flow velocity of 80-120ml/min and controls reaction temperature for 20-30 DEG C, obtains solution B;
Described step S400 specifically refers to: described solution B continues to stir 20-40min, separates out solid, after Separation of Solid and Liquid, gets solids wash, drying, obtain pure, dry silver powder.
The present invention compared with prior art, has the following advantages and beneficial effect:
(1) a kind of silver powder preparation technology controlling particle diameter by controlling NaOH addition provided by the invention, adopts glucose as reducing agent, without toxic residua in production waste liquid, is conducive to environmental protection;
(2) a kind of silver powder preparation technology controlling particle diameter by controlling NaOH addition provided by the invention, controlled the average grain diameter of silver powder by the dosage controlling NaOH, silver powder particle size range is narrow, stable performance;
(3) a kind of silver powder preparation technology controlling particle diameter by controlling NaOH addition provided by the invention, the mass ratio of adjustment silver nitrate crystal and NaOH and adjustable finally prepare the particle diameter of silver powder, simple to operate;
(4) through actual production certification, the output that the present invention prepares silver powder is high.
Accompanying drawing explanation
The stereoscan photograph of silver powder under 10000 times of Fig. 1 to be average grain diameter prepared by preparation technology of the present invention be 0.6-0.9um.
The stereoscan photograph of silver powder under 5000 times of Fig. 2 to be average grain diameter prepared by preparation technology of the present invention be 0.9-1.5um.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
Embodiment 1:
A kind of silver powder preparation technology controlling particle diameter by controlling NaOH addition in the present embodiment, comprises the following steps:
Step S100: get silver nitrate crystal respectively and prepare liquor argenti nitratis ophthalmicus, gets NaOH crystal preparation sodium hydroxide solution, gets glucose crystal preparation glucose solution; Comprise following concrete steps:
Step S110: the silver nitrate crystal adding 80000g in 83L deionized water, is constantly stirred to whole dissolving, obtains liquor argenti nitratis ophthalmicus;
Step S120: the NaOH crystal adding 37300-42504g in 240L deionized water, is constantly stirred to whole dissolving, obtains sodium hydroxide solution;
Step S130: the glucose crystal adding 6664g in 14.4L hot deionized water, is constantly stirred to whole dissolving, obtains glucose solution;
Step S200: under stirring, described liquor argenti nitratis ophthalmicus adds in described sodium hydroxide solution with the flow velocity of 1600ml/min, continues to stir, and obtains solution A;
Step S300: under stirring, described glucose solution adds described solution A with the flow velocity of 100ml/min and controls reaction temperature for 20-30 DEG C, obtains solution B;
Step S400: described solution B continues to stir 30min, separates out solid, after Separation of Solid and Liquid, gets solids wash, drying, obtain pure, dry silver powder.
In the present embodiment, silver powder preparation technology prepares the average grain diameter of silver powder is 0.6-2.2um.
Addition by controlling NaOH in the present invention controls the pH value of solution A, and by the impact of pH value on reduction reaction rate in step S300, control the scope generating silver powder particles particle diameter: when step S300 and glucose mix with solution A and reacts, the pH value of mixed solution is larger, the reproducibility of glucose is stronger, the speed of reduction reaction is faster, and the particle diameter generating silver powder particles is less; Otherwise when step S300 and glucose mix with solution A and reacts, the pH value of mixed solution is less, and the reproducibility of glucose is more weak, and the speed of reduction reaction is slower, the particle diameter generating silver powder particles is larger.
Embodiment 2:
The present embodiment does further optimization on the basis of embodiment 1, and a kind of silver powder preparation technology controlling particle diameter by controlling NaOH addition, comprises the following steps:
Step S100: get silver nitrate crystal respectively and prepare liquor argenti nitratis ophthalmicus, gets NaOH crystal preparation sodium hydroxide solution, gets glucose crystal preparation glucose solution; Comprise following concrete steps:
Step S110: the silver nitrate crystal adding 80000g in 83L deionized water, is constantly stirred to whole dissolving, obtains liquor argenti nitratis ophthalmicus;
Step S120: the NaOH crystal adding 42504g in 240L deionized water, is constantly stirred to whole dissolving, obtains sodium hydroxide solution;
Step S130: the glucose crystal adding 6664g in 14.4L hot deionized water, is constantly stirred to whole dissolving, obtains glucose solution;
Step S200: under stirring, described liquor argenti nitratis ophthalmicus adds in described sodium hydroxide solution with the flow velocity of 1600ml/min, continues to stir, and obtains solution A;
Step S300: under stirring, described glucose solution adds described solution A with the flow velocity of 100ml/min and controls reaction temperature for 20-30 DEG C, obtains solution B;
Step S400: described solution B continues to stir 30min, separates out solid, after Separation of Solid and Liquid, gets solids wash, drying, obtain pure, dry silver powder.
As shown in Figure 1, the average grain diameter of silver powder is 0.6-0.9um, and tap density is 0.8-1.6g/cm
3, specific area is 0.7-1.4m
2/ g.
Embodiment 3:
The present embodiment does further optimization on the basis of embodiment 1, and a kind of silver powder preparation technology controlling particle diameter by controlling NaOH addition, comprises the following steps:
Step S100: get silver nitrate crystal respectively and prepare liquor argenti nitratis ophthalmicus, gets NaOH crystal preparation sodium hydroxide solution, gets glucose crystal preparation glucose solution; Comprise following concrete steps:
Step S110: the silver nitrate crystal adding 80000g in 83L deionized water, is constantly stirred to whole dissolving, obtains liquor argenti nitratis ophthalmicus;
Step S120: the NaOH crystal adding 40572g in 240L deionized water, is constantly stirred to whole dissolving, obtains sodium hydroxide solution;
Step S130: the glucose crystal adding 6664g in 14.4L hot deionized water, is constantly stirred to whole dissolving, obtains glucose solution;
Step S200: under stirring, described liquor argenti nitratis ophthalmicus adds in described sodium hydroxide solution with the flow velocity of 1600ml/min, continues to stir, and obtains solution A;
Step S300: under stirring, described glucose solution adds described solution A with the flow velocity of 100ml/min and controls reaction temperature for 20-30 DEG C, obtains solution B;
Step S400: described solution B continues to stir 30min, separates out solid, after Separation of Solid and Liquid, gets solids wash, drying, obtain pure, dry silver powder.
As shown in Figure 2, the average grain diameter of silver powder is 0.9-1.5um, and tap density is 1.3-2.0g/cm
3, specific area is 0.5-1.0m
2/ g.
Embodiment 4:
The present embodiment does further optimization on the basis of embodiment 1, and a kind of silver powder preparation technology controlling particle diameter by controlling NaOH addition, comprises the following steps:
Step S100: get silver nitrate crystal respectively and prepare liquor argenti nitratis ophthalmicus, gets NaOH crystal preparation sodium hydroxide solution, gets glucose crystal preparation glucose solution; Comprise following concrete steps:
Step S110: the silver nitrate crystal adding 80000g in 83L deionized water, is constantly stirred to whole dissolving, obtains liquor argenti nitratis ophthalmicus;
Step S120: the NaOH crystal adding 37300g in 240L deionized water, is constantly stirred to whole dissolving, obtains sodium hydroxide solution;
Step S130: the glucose crystal adding 6664g in 14.4L hot deionized water, is constantly stirred to whole dissolving, obtains glucose solution;
Step S200: under stirring, described liquor argenti nitratis ophthalmicus adds in described sodium hydroxide solution with the flow velocity of 1600ml/min, continues to stir, and obtains solution A;
Step S300: under stirring, described glucose solution adds described solution A with the flow velocity of 100ml/min and controls reaction temperature for 20-30 DEG C, obtains solution B;
Step S400: described solution B continues to stir 30min, separates out solid, after Separation of Solid and Liquid, gets solids wash, drying, obtain pure, dry silver powder.
The average grain diameter of silver powder is 1.5-2.2um, and tap density is 2.2-2.8g/cm
3, specific area is 0.3-0.8m
2/ g.
Embodiment 5:
A kind of silver powder preparation technology controlling particle diameter by controlling NaOH addition of the present embodiment, is mainly achieved through the following technical solutions: comprise the following steps:
Step S100: get silver nitrate crystal respectively and prepare liquor argenti nitratis ophthalmicus, gets NaOH crystal preparation sodium hydroxide solution, gets glucose crystal preparation glucose solution;
Step S200: under stirring, slowly adds described liquor argenti nitratis ophthalmicus in described sodium hydroxide solution, obtains solution A;
Step S300: be under the condition of 20-30 DEG C in reaction temperature, slowly adds described glucose solution in described solution A and is also constantly stirred to complete reaction, obtain solution B;
Step S400: after described solution B is continued to stir a period of time, Separation of Solid and Liquid, gets solids wash, drying, obtain silver powder.
Can prepare the different silver powder of average grain diameter by adjustment silver nitrate crystal from the mass ratio of NaOH crystal in preparation technology of the present invention, and the silver powder average particle size range of preparation is narrow, performance is very close.
Embodiment 6:
The present embodiment does further optimization on the basis of embodiment 5, and a kind of silver powder preparation technology controlling particle diameter by controlling NaOH addition, comprises the following steps:
Step S100: get silver nitrate crystal respectively and prepare liquor argenti nitratis ophthalmicus, gets NaOH crystal preparation sodium hydroxide solution, gets glucose crystal preparation glucose solution; Described step S100 specifically comprises the following steps:
Step S110: add silver nitrate crystal in deionized water, is constantly stirred to whole dissolving, obtains liquor argenti nitratis ophthalmicus;
Step S120: add NaOH crystal in deionized water, is constantly stirred to whole dissolving, obtains sodium hydroxide solution;
Step S130: be add glucose crystal in the hot deionized water of 40-50 DEG C to temperature, be constantly stirred to whole dissolving, obtain glucose solution;
Step S200: under stirring, described liquor argenti nitratis ophthalmicus adds in described sodium hydroxide solution with the flow velocity of 1500-1700ml/min, continues to stir, and obtains solution A;
Step S300: under stirring, described glucose solution adds described solution A with the flow velocity of 70-130ml/min, obtains solution B;
Step S400: described solution B continues to stir a period of time, separates out solid, after Separation of Solid and Liquid, gets solids wash, drying, obtain pure, dry silver powder.
Embodiment 7:
The present embodiment does further optimization on the basis of embodiment 5, the technique preparing silver powder is: the silver nitrate crystal and the NaOH crystal that first weigh certain mass ratio respectively, prepare liquor argenti nitratis ophthalmicus by described step S110, prepare sodium hydroxide solution by described step S120, take appropriate glucose crystal simultaneously and prepare glucose solution by described step S130; Then by described step S200, the liquor argenti nitratis ophthalmicus prepared respectively is added sodium hydroxide solution while stirring slowly, obtain solution A; Continue by described step S300, the glucose solution of preparation to be stirred while slowly add in described solution A, obtain solution B; Finally solution B is continued to be stirred to precipitation solid, gets solids wash, drying, pure, dry silver powder particles.
When the mass ratio of silver nitrate crystal and NaOH crystal is 1:0.46-0.54, the average grain diameter of obtained silver powder is 0.6-2.2um.Concrete, when the mass ratio of silver nitrate crystal and NaOH crystal is 1:0.46, the average grain diameter of obtained silver powder is 1.5-2.2um; When the mass ratio of silver nitrate crystal and NaOH crystal is 1:0.51, the average grain diameter of obtained silver powder is 0.9-1.5um; When the mass ratio of silver nitrate crystal and NaOH crystal is 1:0.46, the average grain diameter of obtained silver powder is 0.6-0.9um.
Other parts of the present embodiment are identical with embodiment 5, therefore repeat no more.
Embodiment 8:
A kind of silver powder preparation technology controlling particle diameter by controlling NaOH addition of the present embodiment, is mainly achieved through the following technical solutions: comprise the following steps:
Step S100: get silver nitrate crystal respectively and prepare liquor argenti nitratis ophthalmicus, gets NaOH crystal preparation sodium hydroxide solution, gets glucose crystal preparation glucose solution.
Described step S100 specifically comprises the following steps:
Step S110: add silver nitrate crystal in deionized water, is constantly stirred to whole dissolving, obtains liquor argenti nitratis ophthalmicus;
Step S120: add NaOH crystal in deionized water, is constantly stirred to whole dissolving, obtains sodium hydroxide solution;
Step S130: add glucose crystal in hot deionized water, is constantly stirred to whole dissolving, obtains glucose solution.
Step S110 specifically refers to: the silver nitrate crystal adding 80000g in 83L deionized water, is constantly stirred to whole dissolving, obtains liquor argenti nitratis ophthalmicus.
Step S120 specifically refers to: in 240L deionized water, add quantitative NaOH crystal, be constantly stirred to whole dissolving, obtain sodium hydroxide solution.
Step S130 specifically refers to: the glucose crystal adding 6664g in 14.4L hot deionized water, is constantly stirred to whole dissolving, obtains glucose solution.
Hot deionized water in described step S130 refers to that temperature is the deionized water of 40-50 DEG C.
Step S200: under stirring, slowly adds described liquor argenti nitratis ophthalmicus in described sodium hydroxide solution, obtains solution A.
Described step S200 specifically refers to: under stirring, and described liquor argenti nitratis ophthalmicus adds in described sodium hydroxide solution with the flow velocity of 1500-1700ml/min, continues to stir, and obtains solution A.
Step S300: be under the condition of 20-30 DEG C in reaction temperature, slowly adds described glucose solution in described solution A and is also constantly stirred to complete reaction, obtain solution B.
Described step S300 specifically refers to: under stirring, and described glucose solution adds described solution A with the flow velocity of 70-130ml/min, obtains solution B.
Step S400: after described solution B is continued to stir a period of time, Separation of Solid and Liquid, gets solids wash, drying, obtain silver powder.
Described step S400 specifically refers to: described solution B continues to stir 20-40min, separates out solid, after Separation of Solid and Liquid, gets solids wash, drying, obtain pure, dry silver powder.
The solid of separating out in described step S400, first with deionized water and ethanol alternately washing, then low temperature drying.
Described washing specifically comprises the following steps:
Step S411: carry out first pass washing by deionized water;
Step S412: carry out second time washing with ethanol;
Step S413: carry out the 3rd time washing by deionized water;
Step S414: carry out the 4th time washing with ethanol;
Step S415: carry out the 5th time washing by deionized water;
Step S416: carry out the 6th time washing with ethanol.
Described drying specifically refer to by: the drying baker of 60-80 DEG C put into by the silver powder after washing, baking 4-12h.
Described drying can be carried out in vacuum drying chamber, specifically refers to: the silver powder after washing is put into vacuum drying chamber, is 0.7*10 by mechanical pump extracting air to vacuum
-3pa-0.9*10
-3pa, and then make baking temperature in vacuum drying chamber slowly be increased to 60-80 DEG C, continue baking 4-12h, obtain pure, dry silver powder.By the silver powder after washing, be 0.8*10 in vacuum
-3pa, temperature are under the environment of 70 DEG C, and baking 6h, can obtain pure, dry silver powder particles.
When the mass ratio of described silver nitrate crystal and NaOH crystal is 1:0.46-0.54, obtained average grain diameter is the silver powder of 0.6-2.2um.
When the mass ratio of described silver nitrate crystal and NaOH crystal is 1:0.46, obtained average grain diameter is the silver powder of 1.5-2.2um.
When the mass ratio of described silver nitrate crystal and NaOH crystal is 1:0.51, obtained average grain diameter is the silver powder of 0.9-1.5um.
When the mass ratio of described silver nitrate crystal and NaOH crystal is 1:0.54, obtained average grain diameter is the silver powder of 0.6-0.9um.
Embodiment 9:
A kind of silver powder preparation technology controlling particle diameter by controlling NaOH addition in the present embodiment, comprises the following steps:
Step S100: take liquor argenti nitratis ophthalmicus that mass ratio is 1:0.46-0.54:0.0833, sodium hydroxide solution, glucose solution produce corresponding solution respectively; Specifically comprise the following steps:
Step S110: add 1 part of silver nitrate crystal in deionized water, be constantly stirred to whole dissolving, obtain liquor argenti nitratis ophthalmicus;
Step S120: add 0.46-0.54 part NaOH crystal in deionized water, be constantly stirred to whole dissolving, obtain sodium hydroxide solution;
Step S130: add 0.0833 part of glucose crystal in hot deionized water, be constantly stirred to whole dissolving, obtain glucose solution;
Step S200: under stirring, described liquor argenti nitratis ophthalmicus adds in described sodium hydroxide solution with the flow velocity of 1550-1650ml/min, continues to stir 10-40min, obtains solution A;
Step S300: under stirring, described glucose solution adds described solution A with the flow velocity of 80-120ml/min, obtains solution B;
Step S400: described solution B continues to stir 25-35min, separates out solid, after Separation of Solid and Liquid, gets solids wash, drying, obtain pure, dry silver powder.
The solid of separating out in described step S400, first with deionized water and ethanol alternately washing, then low temperature drying.Described washing specifically comprises the following steps:
Step S411: carry out first pass washing by deionized water;
Step S412: carry out second time washing with ethanol;
Step S413: carry out the 3rd time washing by deionized water;
Step S414: carry out the 4th time washing with ethanol;
Step S415: carry out the 5th time washing by deionized water;
Step S416: carry out the 6th time washing with ethanol.
Described drying specifically refer to by: the drying baker of 60-80 DEG C put into by the silver powder after washing, baking 4-12h.
Embodiment 10:
Controlling a silver powder preparation technology for particle diameter by controlling NaOH addition, comprising the following steps:
Step S100: take liquor argenti nitratis ophthalmicus that mass ratio is 1:0.46:0.0833, sodium hydroxide solution, glucose solution produce corresponding solution respectively; Specifically comprise the following steps:
Step S110: add 1 part of silver nitrate crystal in deionized water, be constantly stirred to whole dissolving, obtain liquor argenti nitratis ophthalmicus;
Step S120: add 0.46 part of NaOH crystal in deionized water, be constantly stirred to whole dissolving, obtain sodium hydroxide solution;
Step S130: add 0.0833 part of glucose crystal in hot deionized water, be constantly stirred to whole dissolving, obtain glucose solution;
Step S200: under stirring, described liquor argenti nitratis ophthalmicus adds in described sodium hydroxide solution with the flow velocity of 1650ml/min, continues to stir 15min, obtains solution A;
Step S300: under stirring, described glucose solution adds described solution A with the flow velocity of 120ml/min, obtains solution B;
Step S400: described solution B continues to stir 30min, separates out solid, after Separation of Solid and Liquid, gets solids wash, drying, obtain that average grain diameter is 1.5-2.2um, pure, dry silver powder.
The solid of separating out in described step S400, first with deionized water and ethanol alternately washing, then low temperature drying.Described washing specifically comprises the following steps:
Step S411: carry out first pass washing by deionized water;
Step S412: carry out second time washing with ethanol;
Step S413: carry out the 3rd time washing by deionized water;
Step S414: carry out the 4th time washing with ethanol;
Step S415: carry out the 5th time washing by deionized water;
Step S416: carry out the 6th time washing with ethanol.
Described drying specifically refer to by: the drying baker of 65 DEG C put into by the silver powder after washing, baking 7h.
Embodiment 11:
Controlling a silver powder preparation technology for particle diameter by controlling NaOH addition, comprising the following steps:
Step S100: take liquor argenti nitratis ophthalmicus that mass ratio is 1:0.51:0.0833, sodium hydroxide solution, glucose solution produce corresponding solution respectively; Specifically comprise the following steps:
Step S110: add 1 part of silver nitrate crystal in deionized water, be constantly stirred to whole dissolving, obtain liquor argenti nitratis ophthalmicus;
Step S120: add 0.51 part of NaOH crystal in deionized water, be constantly stirred to whole dissolving, obtain sodium hydroxide solution;
Step S130: add 0.0833 part of glucose crystal in hot deionized water, be constantly stirred to whole dissolving, obtain glucose solution;
Step S200: under stirring, described liquor argenti nitratis ophthalmicus adds in described sodium hydroxide solution with the flow velocity of 1600ml/min, continues to stir 30min, obtains solution A;
Step S300: under stirring, described glucose solution adds described solution A with the flow velocity of 90ml/min, obtains solution B;
Step S400: described solution B continues to stir 30min, separates out solid, after Separation of Solid and Liquid, gets solids wash, drying, obtain pure, dry silver powder.
The solid of separating out in described step S400, first with deionized water and ethanol alternately washing, then low temperature drying.Described washing specifically comprises the following steps:
Step S411: carry out first pass washing by deionized water;
Step S412: carry out second time washing with ethanol;
Step S413: carry out the 3rd time washing by deionized water;
Step S414: carry out the 4th time washing with ethanol;
Step S415: carry out the 5th time washing by deionized water;
Step S416: carry out the 6th time washing with ethanol.
Described drying specifically refer to by: the drying baker of 70 DEG C put into by the silver powder after washing, baking 7h.
Embodiment 12:
Controlling a silver powder preparation technology for particle diameter by controlling NaOH addition, comprising the following steps:
Step S100: take liquor argenti nitratis ophthalmicus that mass ratio is 1:0.53:0.0833, sodium hydroxide solution, glucose solution produce corresponding solution respectively; Specifically comprise the following steps:
Step S110: add 1 part of silver nitrate crystal in deionized water, be constantly stirred to whole dissolving, obtain liquor argenti nitratis ophthalmicus;
Step S120: add 0.53 part of NaOH crystal in deionized water, be constantly stirred to whole dissolving, obtain sodium hydroxide solution;
Step S130: add 0.0833 part of glucose crystal in hot deionized water, be constantly stirred to whole dissolving, obtain glucose solution;
Step S200: under stirring, described liquor argenti nitratis ophthalmicus adds in described sodium hydroxide solution with the flow velocity of 1750ml/min, continues to stir 30min, obtains solution A;
Step S300: under stirring, described glucose solution adds described solution A with the flow velocity of 90ml/min, obtains solution B;
Step S400: described solution B continues to stir 30min, separates out solid, after Separation of Solid and Liquid, gets solids wash, drying, obtain pure, dry silver powder.
The solid of separating out in described step S400, first with deionized water and ethanol alternately washing, then low temperature drying.Described washing specifically comprises the following steps:
Step S411: carry out first pass washing by deionized water;
Step S412: carry out second time washing with ethanol;
Step S413: carry out the 3rd time washing by deionized water;
Step S414: carry out the 4th time washing with ethanol;
Step S415: carry out the 5th time washing by deionized water;
Step S416: carry out the 6th time washing with ethanol.
Described drying specifically refer to by: the drying baker of 65 DEG C put into by the silver powder after washing, baking 7h.
The above is only preferred embodiment of the present invention, and not do any pro forma restriction to the present invention, every any simple modification, equivalent variations done above embodiment according to technical spirit of the present invention, all falls within protection scope of the present invention.
Claims (10)
1. controlling a silver powder preparation technology for particle diameter by controlling NaOH addition, it is characterized in that: controlling by controlling the silver powder particle diameter of NaOH addition to preparation, specifically comprising the following steps:
Step S100: get silver nitrate crystal respectively and prepare liquor argenti nitratis ophthalmicus, gets NaOH crystal preparation sodium hydroxide solution, gets glucose crystal preparation glucose solution;
Step S200: under stirring, slowly adds described liquor argenti nitratis ophthalmicus in described sodium hydroxide solution, obtains solution A;
Step S300: be under the condition of 20-30 DEG C in reaction temperature, slowly adds described glucose solution in described solution A and is also constantly stirred to complete reaction, obtain solution B;
Step S400: after described solution B is continued to stir a period of time, Separation of Solid and Liquid, gets solids wash, drying, obtain silver powder.
2. a kind of silver powder preparation technology controlling particle diameter by controlling NaOH addition according to claim 1, is characterized in that: in described step S100, the mass ratio of silver nitrate crystal and NaOH crystal is 1:0.46-0.54; In described step S400, the average grain diameter of obtained silver powder is 0.6-2.2um.
3. a kind of silver powder preparation technology controlling particle diameter by controlling NaOH addition according to claim 2, it is characterized in that: when the mass ratio of described silver nitrate crystal and NaOH crystal is 1:0.46, obtained average grain diameter is the silver powder of 1.5-2.2um.
4. a kind of silver powder preparation technology controlling particle diameter by controlling NaOH addition according to claim 2, it is characterized in that: when the mass ratio of described silver nitrate crystal and NaOH crystal is 1:0.51, obtained average grain diameter is the silver powder of 0.9-1.5um.
5. a kind of silver powder preparation technology controlling particle diameter by controlling NaOH addition according to claim 2, it is characterized in that: when the mass ratio of described silver nitrate crystal and NaOH crystal is 1:0.54, obtained average grain diameter is the silver powder of 0.6-0.9um.
6. a kind of silver powder preparation technology controlling particle diameter by controlling NaOH addition according to any one of claim 1-5, is characterized in that: described step S100 specifically comprises the following steps:
Step S110: add silver nitrate crystal in deionized water, is constantly stirred to whole dissolving, obtains liquor argenti nitratis ophthalmicus;
Step S120: add NaOH crystal in deionized water, is constantly stirred to whole dissolving, obtains sodium hydroxide solution;
Step S130: add glucose crystal in hot deionized water, is constantly stirred to whole dissolving, obtains glucose solution.
7. a kind of silver powder preparation technology controlling particle diameter by controlling NaOH addition according to any one of claim 1-5, it is characterized in that: described step S200 specifically refers to: under stirring, described liquor argenti nitratis ophthalmicus adds in described sodium hydroxide solution with the flow velocity of 1500-1700ml/min, continue to stir, obtain solution A.
8. a kind of silver powder preparation technology controlling particle diameter by controlling NaOH addition according to any one of claim 1-5, it is characterized in that: described step S300 specifically refers to: under stirring, described glucose solution adds described solution A with the flow velocity of 70-130ml/min, obtains solution B.
9. a kind of silver powder preparation technology controlling particle diameter by controlling NaOH addition according to any one of claim 1-5, it is characterized in that: described step S400 specifically refers to: described solution B continues to stir a period of time, separate out solid, after Separation of Solid and Liquid, get solids wash, drying, obtain pure, dry silver powder.
10. a kind of silver powder preparation technology controlling particle diameter by controlling NaOH addition according to any one of claim 1-5, is characterized in that:
Described step S100 specifically comprises the following steps:
Step S110: the silver nitrate crystal adding 80000g in 83L deionized water, is constantly stirred to whole dissolving, obtains liquor argenti nitratis ophthalmicus;
Step S120: add quantitative NaOH crystal in 240L deionized water, be constantly stirred to whole dissolving, obtain sodium hydroxide solution;
Step S130: the glucose crystal adding 6664g in 14.4L hot deionized water, is constantly stirred to whole dissolving, obtains glucose solution;
Described step S200 specifically refers to: under stirring, and described liquor argenti nitratis ophthalmicus adds in described sodium hydroxide solution with the flow velocity of 1550-1650ml/min, continues to stir, and obtains solution A;
Described step S300 specifically refers to: under stirring, and described glucose solution adds described solution A with the flow velocity of 80-120ml/min and controls reaction temperature for 20-30 DEG C, obtains solution B;
Described step S400 specifically refers to: described solution B continues to stir 20-40min, separates out solid, after Separation of Solid and Liquid, gets solids wash, drying, obtain pure, dry silver powder.
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