CN109014239A - A kind of preparation method of touch screen laser ablation silver paste silver powder - Google Patents
A kind of preparation method of touch screen laser ablation silver paste silver powder Download PDFInfo
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- CN109014239A CN109014239A CN201810886037.7A CN201810886037A CN109014239A CN 109014239 A CN109014239 A CN 109014239A CN 201810886037 A CN201810886037 A CN 201810886037A CN 109014239 A CN109014239 A CN 109014239A
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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
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Abstract
The invention discloses a kind of touch screen preparation methods of laser ablation silver paste silver powder, belong to conductive metal Preparation Technique of Powders field, include the following steps: to prepare reducing agent solution, dispersant solution and metal salt solution, hybrid reaction, washing is separated by solid-liquid separation to obtain filter cake to conductivity≤20ms, and filter cake is dried to moisture content and obtains silver powder less than 0.2%.Preparation method of the invention is easy to operate, and raw material sources are extensive, at low cost, to the of less demanding of equipment；Obtained touch screen is very high with the diameter of particle concentration degree of the preparation method of laser ablation silver paste silver powder, silver powder maximum particle diameter D1005 μm of <, good dispersion.
Description
Technical field
The invention belongs to conductive metal Preparation Technique of Powders fields, and in particular to a kind of touch screen laser ablation silver paste use
The preparation method of silver powder.
Background technique
Touch screen originates from the U.S. of the 1960s, is that US military is developed for military use.More than 50
The development in year, touch screen has been widely used, but just actually enters the maturity period after 2000.The first generation in 2007
IPhone mobile phone has pulled open the prelude in smart phone full touch-control epoch, becomes a milestone of touch-control industry development.2010
Year, with the explosive growth of smart phone and being announced to the world splendidly for tablet computer, touch control operation, especially capacitance touching control are operated
Core status on intelligent mobile terminal is confirmed.First generation iPad publication, so that touch screen competition is extended from small size
To middle large size product market.2012, Samsung emerged in smart phone market, while tablet computer enters the fast growth phase,
The heating of ultrabook concept, touch screen field enters the high-speed developing period of product diversification, brand diversification.
Currently, with the continuous development of science and technology, touch screen will be used wider and wider.It is operated from the control of shop equipment
System, the electronic equipment of public information inquiry, commercial use ATM, arrive consumer electronics mobile phone, PDA, numerical control phase
The figure of touch screen all can be seen in machine etc..According to the related data of market research agency Display Search, the whole world in 2016
Touch screen shipment amount reaches 3,000,000,000 pieces, and business revenue reaches 30,000,000,000 dollars, and the development prospect in touch screen market future is very tempting.But
When smart electronic consumer product mobile phone, tablet computer etc. become the carrier of universal information transmission and reading, carrying user information is got over
While coming more, people put forward higher requirements touch-control industry again.The electrode silver of one of critical material as touch screen
Slurry, it is most direct on touch screen performance influence, and as the requirement for touching precision is higher and higher, silver paste also proposed higher more
Harsh technical requirements.
However, the silver paste and silver powder product of mating touch screen domestic at present are almost blank, 95% or more all rely on into
Mouthful.And have two side's production methods at present for touch screen silver paste electrode circuit, first is that using traditional silk-screen printing technique in ITO
Surface printing electronic circuit, this is current preparation contact electrode and the widely used technology of conducting wire；Second is that being lost by laser
It carves, the touch screen made using laser ablation is linear preferably, without extra burr phenomena, without bad appearance defect hidden danger, and swashs
Photoetch has the characteristics such as non-contact, pollution-free, easy to control, is the important application skill of current conductive paste stockline etching width control
Art.Since the conducting wire track using silk-screen printing technique is wider than 50 microns, and it is of less demanding to the dispersibility of silver powder, this
Class silver powder has realized production domesticization at present；And as touch screen is thinner and lighter, the development of multi-touch function, to silver wire conducting wire cloth
Line density proposes requirements at the higher level (20-30 μm of conductive line width), has exceeded the limitation of traditional silk-screened technology, therefore to silver powder
More stringent requirements are proposed, that is, requires that the particle size range of silver powder is narrow, dispersion performance is good, is not allow for the presence of bulky grain silver powder,
Otherwise it will affect the yields of touch screen, and the silver powder of China's laser-induced thermal etching has 90% or more to rely on import.
Summary of the invention
The object of the present invention is to provide a kind of touch screen preparation methods of laser ablation silver paste silver powder, to solve silver powder
The more difficult concentration of partial size, size particles are unable to control, the bad problem of the dispersibility of silver powder.
In order to achieve the above object, the technical solution adopted by the present invention are as follows:
A kind of preparation method of touch screen laser ablation silver paste silver powder, it is characterised in that include the following steps:
Step 1: dissolving reduce agent in pure water, reducing agent solution A is obtained, temperature adjustment is to 45 ± 5 DEG C；
Step 2: dispersing agent is dissolved in pure water, adds alkali to adjust pH value to 12.0-13.0, obtain dispersant solution B, temperature adjustment is extremely
45±5℃；
Metal salt solution C is obtained Step 3: silver nitrate is dissolved in pure water, temperature adjustment is to 45 ± 5 DEG C；
Step 4: the dispersant solution B that step 2 the obtains and metal salt solution C that step 3 obtains is added what step 1 obtained
It is stirred in reducing agent solution A, reacts 3-5min；
Step 5: being filtered after separation of solid and liquid when the mixed solution that step 4 is obtained is washed to filtered solution conductivity≤20ms
Hydrophobicity auxiliary agent is added in filter cake, terminates to be dried to obtain silver powder when being dried to moisture content less than 0.2% for cake.
Reducing agent described in step 1 is formic acid, ascorbic acid, formaldehyde or hydrazine hydrate.
Alkali described in step 2 is sodium hydroxide, ammonium hydroxide or carbonic acid sodium.
Dispersing agent described in step 2 is benzotriazole acid, polyvinylpyrrolidone or Tween-80.
The concentration of silver nitrate described in step 3 is 600g/L-650g/L.
Step 1: reducing agent solution described in two, three, dispersant solution, silver nitrate solution temperature are 45 DEG C, it is to guarantee
Reaction system initial temperature is 45 DEG C.Reaction temperature is higher than silver powder prepared by this temperature and is easy to reunite, and is lower than this thermotonus
It is difficult to carry out completely.
Dispersant solution B described in step 4 and metal salt solution C are the reducing agent solution A being quickly poured under stirring
In, the molar ratio of reducing agent and silver nitrate in the reducing agent solution A is 2:1-4:1, the dispersing agent in dispersant solution B with
The molar ratio of silver nitrate is 0.01:1-0.05:1.
Hydrophobicity auxiliary agent described in step 5 is isomery stearic acid, hexadecanol, oleic acid or lauric acid, and hydrophobicity auxiliary agent is added
Amount and the molar ratio of silver nitrate are 0.01:1-0.05:1.
The dispersant solution B and metal salt solution C time that reducing agent solution A is added is controlled in 10s described in step 4
It is interior.
The present invention having the beneficial effect that compared to the prior art
The present invention, which is used, adds dispersing agent into reducing agent solution, and adjusts reduction system pH value by the way that alkali is added to restore
Metal salt solution C, obtains silver powder.The selection of reducing agent is satisfactory to obtain size in order to preferably control reaction rate
Silver powder particles, the selection of dispersing agent are that silver powder is reunited during the preparation process in order to prevent, influence the pattern and physics and chemistry of silver powder
Index, while the pH of reduction system is controlled, to guarantee the best use effect of reducing agent and dispersing agent, finally prepare silver powder grain
Diameter is concentrated, size particles are controllable, silver powder good dispersion reaches acquisition crystallinity by control silver powder forming core and growth rate
The purpose of high, homogeneous grain diameter silver powder product.
Preparation method of the invention is easy to operate, and raw material sources are extensive, at low cost, to the of less demanding of equipment；It obtains
Touch screen is very high with the diameter of particle concentration degree of the preparation method of laser ablation silver paste silver powder, silver powder maximum particle diameter D1005 μ of <
M, good dispersion.
Specific embodiment
The present invention will be further described With reference to embodiment.
A kind of touch screen preparation method of laser ablation silver paste silver powder, includes the following steps:
Step 1: dissolving reduce agent in pure water, reducing agent solution A is obtained, temperature adjustment is to 45 ± 5 DEG C；
Step 2: dispersing agent is dissolved in pure water, adds alkali to adjust pH value to 12.0-13.0, obtain dispersant solution B, temperature adjustment is extremely
45±5℃；
Metal salt solution C is obtained Step 3: silver nitrate is dissolved in pure water, temperature adjustment is to 45 ± 5 DEG C；
Step 4: the dispersant solution B that step 2 the obtains and metal salt solution C that step 3 obtains is added what step 1 obtained
It is stirred in reducing agent solution A, reacts 3-5min；
Step 5: being filtered after separation of solid and liquid when the mixed solution that step 4 is obtained is washed to filtered solution conductivity≤20ms
Hydrophobicity auxiliary agent is added in filter cake, terminates to be dried to obtain silver powder when being dried to moisture content less than 0.2% for cake.
Reducing agent described in step 1 is formic acid, ascorbic acid, formaldehyde or hydrazine hydrate.
Alkali described in step 2 is sodium hydroxide, ammonium hydroxide or carbonic acid sodium.
Dispersing agent described in step 2 is benzotriazole, polyvinylpyrrolidone or Tween-80.
The concentration of silver nitrate described in step 3 is 600g/L-650g/L.
Step 1: reducing agent solution described in two, three, dispersant solution, silver nitrate solution temperature are 45 DEG C, it is to guarantee
Reaction system initial temperature is 45 DEG C.
Dispersant solution B described in step 4 and metal salt solution C are the reducing agent solution A being quickly poured under stirring
In, the molar ratio of reducing agent and silver nitrate in the reducing agent solution A is 2:1-4:1, the dispersing agent in dispersant solution B with
The molar ratio of silver nitrate is 0.01:1-0.05:1.
Hydrophobicity auxiliary agent described in step 5 is isomery stearic acid, hexadecanol, oleic acid or lauric acid, and hydrophobicity auxiliary agent is added
Amount and the molar ratio of silver nitrate are 0.01:1-0.05:1.
The dispersant solution B and metal salt solution C time that reducing agent solution A is added is controlled in 10s described in step 4
It is interior.
Embodiment 1:
It weighs 176.82g hydrazine hydrate and is dissolved in spare in 1L pure water, as reducing agent solution A, temperature adjustment is to 45 DEG C；
Weigh 68g sodium hydroxide, 2.10g benzotriazole acid is dissolved in spare in 1L pure water, as dispersant solution B, temperature adjustment is extremely
45℃；
It weighs 300g silver nitrate and is dissolved in 0.5L water, as metal salt solution C, temperature adjustment is to 45 DEG C；
Dispersant solution B, metal salt solution C are quickly poured into the lower reducing agent solution A of stirring and reacted, is controlled and is poured into the time and exist
It within 10s, and is stirred, dispersant solution B reacts 3min after all pouring into, detect in reaction solution without Ag+When determine reaction
Terminate；
Acquired solution is separated by solid-liquid separation and is filtered, when conductivity≤20ms washed several times to filtered solution, carries out solid-liquid
Separation and filtering, are added 0.95g isomery stearic acid in filter cake Ag powder, 60 DEG C of 16 hours of drying to moisture content less than 0.2% after tie
Beam is dry；
300 mesh sieve of obtained silver powder are sieved, obtain D after screening50It is 3.85 μm, tap density for 0.46 μm, D100
For 3.85g/cm3Touch screen laser ablation silver paste silver powder.
Embodiment 2:
It weighs 527.23g ascorbic acid and is dissolved in spare in 3.2L pure water, as reducing agent solution A, temperature adjustment is to 50 DEG C；
Weigh 216g sodium hydroxide, 1.75g benzotriazole acid be dissolved in it is spare in 3.2L water, extremely as dispersant solution B temperature adjustment
50℃；
It weighs 250g silver nitrate and is dissolved in 0.4 L water, as metal salt solution C, temperature adjustment is to 50 DEG C；
Dispersant solution B, metal salt solution C are quickly poured into the lower reducing agent solution A of stirring and reacted, is controlled and is poured into the time and exist
It within 10s, and is stirred, dispersant solution B reacts 5min after all pouring into, detect in reaction solution without Ag+When determine reaction
Terminate；
Obtained solution is separated by solid-liquid separation and is filtered, when conductivity≤20ms washed several times to filtered solution, consolidate
Liquid separates and filtering, 1.59g isomery stearic acid is added in filter cake Ag powder, after 60 DEG C of 18 hours of drying to moisture content are less than 0.2%
Terminate drying.
300 mesh sieve of obtained silver powder are sieved, obtain D after screening50It is 3.97 μm, jolt ramming for 0.51 μm, D100
Density is 3.15g/cm3Touch screen laser ablation silver paste silver powder.
Embodiment 3:
It weighs 528.40 formic acid and is dissolved in spare in 3L pure water, as reducing agent solution A, temperature adjustment is to 40 DEG C；
Weigh 150g sodium hydroxide, 34.19g benzotriazole acid is dissolved in spare in 2L water, as dispersant solution B, temperature adjustment is extremely
40℃；
It weighs 975g silver nitrate and is dissolved in 1.5L water, as metal salt solution C, temperature adjustment is to 40 DEG C；
Dispersant solution B, metal salt solution C are quickly poured into the lower reducing agent solution A of stirring and reacted, is controlled and is poured into the time and exist
It within 10s, and is stirred, dispersant solution B reacts 5min after all pouring into, detect in reaction solution without Ag+When determine reaction
Terminate；
Obtained solution is separated by solid-liquid separation and is filtered, when conductivity≤20ms washed several times to filtered solution, consolidate
Liquid separation and filtering, are added 6.18g isomery stearic acid in filter cake Ag powder, 60 DEG C drying 20 hours to moisture content less than 0.2% after tie
Beam is dry.
300 mesh sieve of obtained silver powder are sieved, obtain D after screening50It is 3.53 μm, jolt ramming for 0.49 μm, D100
Density is 3.5g/cm3Touch screen laser ablation silver paste silver powder.
Embodiment 4:
It weighs 530.35 formaldehyde and is dissolved in spare in 3L pure water, as reducing agent solution A, temperature adjustment is to 45 DEG C；
Weigh 130g sodium hydroxide, 7.01g benzotriazole acid be dissolved in it is spare in 2L water, as dispersant solution B, temperature adjustment to 45
℃；
It weighs 1000g silver nitrate and is dissolved in 1.7L water, as metal salt solution C, temperature adjustment is to 45 DEG C；
Dispersant solution B, metal salt solution C are quickly poured into the lower reducing agent solution A of stirring and reacted, is controlled and is poured into the time and exist
It within 10s, and is stirred, dispersant solution B reacts 4min after all pouring into, detect in reaction solution without Ag+When determine reaction
Terminate；
Obtained solution is separated by solid-liquid separation and is filtered, when conductivity≤20ms washed several times to filtered solution, consolidate
Liquid separation and filtering, are added 3.16g isomery stearic acid in filter cake Ag powder, 60 DEG C drying 16 hours to moisture content less than 0.2% after tie
Beam is dry.
300 mesh sieve of obtained silver powder are sieved, obtain D after screening50It is 3.13 μm, jolt ramming for 0.43 μm, D100
Density is 2.9g/cm3Touch screen laser ablation silver paste silver powder.
Embodiment 5:
It weighs 588 hydrazine hydrates and is dissolved in spare in 3L pure water, as reducing agent solution A, temperature adjustment is to 45 DEG C；
Weigh 177g sodium bicarbonate, 500g polyvinylpyrrolidone is dissolved in spare in 2L water, as dispersant solution B, temperature adjustment is extremely
45℃；
It weighs 1000g silver nitrate and is dissolved in 1.5 L water, as metal salt solution C, temperature adjustment is to 45 DEG C；
Dispersant solution B, metal salt solution C are quickly poured into the lower reducing agent solution A of stirring and reacted, is controlled and is poured into the time and exist
It within 10s, and is stirred, dispersant solution B reacts 4min after all pouring into, detect in reaction solution without Ag+When determine reaction
Terminate；
Obtained solution is separated by solid-liquid separation and is filtered, when conductivity≤20ms washed several times to filtered solution, consolidate
Liquid separation and filtering, are added 14g hexadecanol in filter cake Ag powder, 60 DEG C drying 16 hours to moisture content less than 0.2% after terminate it is dry
It is dry.
300 mesh sieve of obtained silver powder are sieved, obtain D after screening50It is 2.13 μm, vibration density for 0.5 μm, D100
Degree is 4.5g/cm3Touch screen laser ablation silver paste silver powder.
Embodiment 6:
It weighs 635 formaldehyde and is dissolved in spare in 3L pure water, as reducing agent solution A, temperature adjustment is to 45 DEG C；
Weigh 125g ammonium hydroxide, 50g Tween-80 is dissolved in spare in 2L water, as dispersant solution B, temperature adjustment is to 45 DEG C；
It weighs 1000g silver nitrate and is dissolved in 1.7 L water, as metal salt solution C, temperature adjustment is to 45 DEG C；
Dispersant solution B, metal salt solution C are quickly poured into the lower reducing agent solution A of stirring and reacted, is controlled and is poured into the time and exist
It within 10s, and is stirred, dispersant solution B reacts 4min after all pouring into, detect in reaction solution without Ag+When determine reaction
Terminate；
Obtained solution is separated by solid-liquid separation and is filtered, when conductivity≤20ms washed several times to filtered solution, consolidate
Liquid separation and filtering, are added 33g oleic acid in filter cake Ag powder, 60 DEG C drying 16 hours to moisture content less than 0.2% after terminate drying.
300 mesh sieve of obtained silver powder are sieved, obtain D after screening50It is 4.39 μm, jolt ramming for 0.58 μm, D100
Density is 3.5g/cm3Touch screen laser ablation silver paste silver powder.
Embodiment 7:
It weighs 600 formaldehyde and is dissolved in spare in 3L pure water, as reducing agent solution A, temperature adjustment is to 45 DEG C；
Weigh 150g ammonium hydroxide, 60g Tween-80 is dissolved in spare in 2L water, as dispersant solution B, temperature adjustment is to 45 DEG C；
It weighs 1000g silver nitrate and is dissolved in 1.5 L water, as metal salt solution C, temperature adjustment is to 45 DEG C；
Dispersant solution B, metal salt solution C are quickly poured into the lower reducing agent solution A of stirring and reacted, is controlled and is poured into the time and exist
It within 10s, and is stirred, dispersant solution B reacts 4min after all pouring into, detect in reaction solution without Ag+When determine reaction
Terminate；
Obtained solution is separated by solid-liquid separation and is filtered, when conductivity≤20ms washed several times to filtered solution, consolidate
Liquid separation and filtering, are added 25g lauric acid in filter cake Ag powder, 60 DEG C drying 16 hours to moisture content less than 0.2% after terminate it is dry
It is dry.
300 mesh sieve of obtained silver powder are sieved, obtain D after screening50It is 4.66 μm, jolt ramming for 0.91 μm, D100
Density is 3.57g/cm3Touch screen laser ablation silver paste silver powder.
Claims (8)
1. a kind of touch screen preparation method of laser ablation silver paste silver powder, it is characterised in that include the following steps:
Step 1: dissolving reduce agent in pure water, reducing agent solution A is obtained, temperature adjustment is to 45 ± 5 DEG C；
Step 2: dispersing agent is dissolved in pure water, adds alkali to adjust pH value to 12.0-13.0, obtain dispersant solution B, temperature adjustment is extremely
45±5℃；
Metal salt solution C is obtained Step 3: silver nitrate is dissolved in pure water, temperature adjustment is to 45 ± 5 DEG C；
Step 4: the dispersant solution B that step 2 the obtains and metal salt solution C that step 3 obtains is added what step 1 obtained
It is stirred in reducing agent solution A, reacts 3-5min；
Step 5: being filtered after separation of solid and liquid when the mixed solution that step 4 is obtained is washed to filtered solution conductivity≤20ms
Hydrophobicity auxiliary agent is added in filter cake, terminates to be dried to obtain silver powder when being dried to moisture content less than 0.2% for cake.
2. the touch screen as described in claim 1 preparation method of laser ablation silver paste silver powder, it is characterised in that: step 1
Described in reducing agent be formic acid, ascorbic acid, formaldehyde or hydrazine hydrate.
3. the touch screen as described in claim 1 preparation method of laser ablation silver paste silver powder, it is characterised in that: step 2
Described in alkali be sodium hydroxide, ammonium hydroxide or carbonic acid sodium.
4. the touch screen as described in claim 1 preparation method of laser ablation silver paste silver powder, it is characterised in that: step 2
Described in dispersing agent be benzotriazole acid, polyvinylpyrrolidone or Tween-80.
5. the touch screen as described in claim 1 preparation method of laser ablation silver paste silver powder, it is characterised in that: step 3
Described in silver nitrate concentration be 600g/L-650g/L.
6. the touch screen as described in claim 1 preparation method of laser ablation silver paste silver powder, it is characterised in that: step 4
Described in dispersant solution B and metal salt solution C be quickly poured into stirring under reducing agent solution A in, the reducing agent is molten
The molar ratio of reducing agent and silver nitrate in liquid A is 2:1-4:1, the molar ratio of dispersing agent and silver nitrate in dispersant solution B
For 0.01:1-0.05:1.
7. the touch screen as described in claim 1 preparation method of laser ablation silver paste silver powder, it is characterised in that: step 5
Described in hydrophobicity auxiliary agent be isomery stearic acid, hexadecanol, oleic acid or lauric acid, hydrophobicity promoter addition and silver nitrate rub
You are than being 0.01:1-0.05:1.
8. the touch screen as described in claim 1 preparation method of laser ablation silver paste silver powder, it is characterised in that: step 4
Described in dispersant solution B and metal salt solution the C time that reducing agent solution A is added are controlled in 10s.
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| CN110586959A (en) * | 2019-10-28 | 2019-12-20 | 苏州银瑞光电材料科技有限公司 | Preparation method of flake silver powder with high tap density |
| CN111438369A (en) * | 2019-01-16 | 2020-07-24 | 北京氦舶科技有限责任公司 | Silver powder, preparation method thereof and laser etching silver paste |
| CN112091233A (en) * | 2020-11-19 | 2020-12-18 | 西安宏星电子浆料科技股份有限公司 | Synthesis method of silver nanoparticles |
| CN112974827A (en) * | 2019-12-12 | 2021-06-18 | 长沙理工大学 | Preparation method of spherical silver powder with high tap density and surface wrinkles |
| CN113290252A (en) * | 2021-05-28 | 2021-08-24 | 金川集团股份有限公司 | Preparation method of superfine silver powder with low tap mass and high specific surface |
| CN114951678A (en) * | 2022-04-25 | 2022-08-30 | 金川集团股份有限公司 | Preparation method of spherical superfine silver powder for silver paste on front surface of solar cell |
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| CN113290252A (en) * | 2021-05-28 | 2021-08-24 | 金川集团股份有限公司 | Preparation method of superfine silver powder with low tap mass and high specific surface |
| CN114951678A (en) * | 2022-04-25 | 2022-08-30 | 金川集团股份有限公司 | Preparation method of spherical superfine silver powder for silver paste on front surface of solar cell |
| CN114951678B (en) * | 2022-04-25 | 2023-12-26 | 金川集团股份有限公司 | Preparation method of spherical superfine silver powder for front silver paste of solar cell |
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Application publication date: 20181218 |