CN106398398A - Metal nano conductive ink and preparation method thereof - Google Patents
Metal nano conductive ink and preparation method thereof Download PDFInfo
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- CN106398398A CN106398398A CN201610816163.6A CN201610816163A CN106398398A CN 106398398 A CN106398398 A CN 106398398A CN 201610816163 A CN201610816163 A CN 201610816163A CN 106398398 A CN106398398 A CN 106398398A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/52—Electrically conductive inks
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/30—Inkjet printing inks
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/30—Inkjet printing inks
- C09D11/36—Inkjet printing inks based on non-aqueous solvents
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/30—Inkjet printing inks
- C09D11/38—Inkjet printing inks characterised by non-macromolecular additives other than solvents, pigments or dyes
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- Engineering & Computer Science (AREA)
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- Wood Science & Technology (AREA)
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- General Chemical & Material Sciences (AREA)
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- Inks, Pencil-Leads, Or Crayons (AREA)
Abstract
The invention discloses metal nano conductive ink and a preparation method thereof. The metal nano conductive ink is prepared from, by weight, 10-60wt% of gold, silver and copper nanoparticle powder, 5-20wt% of metallorganics capable of being decomposed at low temperature, 0-1wt% of non-volatile organic components and 20-80wt% of volatile organic components. The preparation method includes: adding by stirring polymer resin or a mixture thereof into high boiling point solvent or a mixture thereof to form a component A; dissolving the metallorganics into low boiling point solvent to form a component B; adding the nanometer particle powder into the cooled component A and then mixing in the component B of a certain volume; subjecting the obtained mixture to grinding, high-speed shearing and three-roller smelting to promote dispersion to form a sticky component C; proportionally adding the high boiling solvent or the mixture thereof or the component A into the component C, and adjusting system viscosity and content of metal nanoparticles to obtain the final metal nano conductive ink. By the arrangement, low-temperature sintering, high conductivity and large-thickness printing can be realized, and the metal nano conductive ink and the preparation method thereof are widely applicable.
Description
Technical field
The invention belongs to chemical field, it is related to a kind of metal nano conductive ink and preparation method thereof, particularly, should
Metal nano conductive ink can be transferred on the base materials such as PET film, art paper by modes such as ink-jet, gravures, dries shape after sintering
Become pattern and the circuit of high connductivity, can once be formed more than 0.5um print thickness, and be smaller than 150 DEG C of low-temperature sinterings, resistivity
As little as 5u Ω cm.
Background technology
Nano material refer in three dimensions at least one-dimensional be in nanoscale scope (1-100nm) or by they make
The material constituting for elementary cell.After macro object subdivided into nanoscale, its optics, calorifics, electricity, magnetics, mechanics
And the property of chemistry aspect will have significant change, can be widely applied to the crowds such as electronics, medicine, chemical industry, military affairs, Aero-Space
Multi-field.Metal nano material such as gold, silver, copper etc. have the performances such as the optics of uniqueness, electricity, therefore in electronics, optics, show
Show, sense, the energy etc. is widely used in field
Traditional ink is a kind of stable colloidal dispersion system, generally by pigment, hard resin, volatile solvent, filling
Material and additive composition.Pigment provides color for traditional ink, and hard resin is film forming matter.Conventional conductive ink is containing micro-
The colloidal dispersion system of meter level conducting particles, can form pattern and the circuit of conduction, extensively should after its drying or high temperature sintering
For fields such as printed circuit board (PCB), photovoltaics.
Conventional conductive ink if low temperature drying, then conducting particles is by physical contact conducting electric current, thus
Resistance is big, and wet and heat ageing resistant performance is not good, and out of doors etc. severe rugged environment application is limited.In order to expand its range of application, past one
As adopt high temperature sintering, organics removal, allow metallic particles particle fusing integral, thus improving electric conductivity and stability.So
And its sintering temperature is generally greater than more than 400 DEG C, it is difficult to meet the application of plastics base electron device and product.
Recently, people to realize low-temperature sintering conduction using metal nanoparticle.But the dispersion of nano-particle is extremely
Difficult, it usually needs substantial amounts of organic matter, otherwise can be unstable in colloidal dispersion, reunite, flocculate and precipitate, finally
Impact uses.But its dispersion is improved using substantial amounts of organic matter, then the presence due to organic matter can affect in low-temperature sintering
Its electric conductivity, or even hinder sintering to merge.
Content of the invention
The present invention is that in solution prior art, metal nanoparticle ink content of organics is high, active ingredient is low, sintering temperature
The shortcomings such as degree is high, print thickness is thin, be particularly introduced into can low-temperature decomposition type metallorganic as metal nanoparticle
Dispersant, realizes the stable dispersion of metal nanoparticle, and decomposition improves melting of metal nanoparticle at low temperature is less than 150 DEG C
Close, thus realizing low-temperature sintering, high connductivity and the printing of big thickness.
A kind of metal nano conductive ink, containing following component：
1) gold, silver in the range of 1-500nm for the particle diameter, copper nano-particle powder, content 10-60wt%；
2) 150 DEG C of metallorganics decomposing, content 5-20wt% can be less than by low temperature；
3) non-volatile organic principle, consumption 0-1wt%；
4) volatilize organic principle, consumption 20-80wt%.
Preferably, gold, silver in the range of 1-500nm for the particle diameter, copper nano-particle powder can be ground using chemical method synthesis, physics
Prepared by mill, explosion method etc..When the metallic nanoparticle period of the day from 11 p.m. to 1 a.m being obtained using chemical method synthesis, need to be by cleaning, centrifugation and precipitation etc.
Technique removes excessive organic matter, to content low less than 1wt%.When the metal nanoparticle with other method preparation such as physical grinding
When, its content of organics also should control less than 1wt%.
Preferential, 150 DEG C of metallorganics decomposing can be less than by low temperature, there is following structure：
M-X1-R-X2,
Wherein：M is gold, silver, copper ion；R is alkyl chain, and for guaranteeing low temperature volatilization decomposition, usual R contains 1-4 carbon atom；
X1 is the functional group connecting metal ion, such as-COO-, and-S- ,-N- etc. can be with the groups of gold, silver, copper ion cooperation；X2 is can
Dispersion gold, silver, the functional group of copper nano-particle, such as-COOH ,-SH ,-NH2, ethylene glycol alcohol ether chain (chain number 1-4), the third two
Alcohol ether chain (chain number 1-4), polyvinylpyrrolidone chain (chain number 1-4).
Preferably, non-volatile organic principle is macromolecule resin；Macromolecule resin used is ethyl cellulose, hydroxypropyl is fine
Dimension element, acrylic resin, polyurethane resin.
Preferably, volatilization organic principle is high boiling solvent, surface modifier.
Preferably, high boiling solvent used is glycol propyl ether, butyl glycol ether, diethylene glycol ether, diethylene glycol third
Ether, butyl, propylene glycol propyl ether, propandiol butyl ether, dipropylene glycol ethyl ether, dipropylene glycol propyl ether, dipropylene,
Glycol propyl ether acetate, 2-Butoxyethyl acetate, diethylene glycol ether acetate, diethylene glycol propyl ether acetate, diethyl
Glycol monobutyl ether acetate, propylene glycol propyl ether acetate, propandiol butyl ether acetate, dipropylene glycol ethyl ether acetate, DPG
Propyl ether acetate, dipropylene acetate, ethylene glycol, terpinol, petroleum ether.
Preferably, surface modifier used is organic amine, organic carboxyl acid, polyethylene oxide and polyoxy propane copolymer, dehydration mountain
Pears alcohol fatty acid ester, sucrose fatty ester, polyoxyethylene aliphatic alcohol ether, poly-for polyoxyethylene fatty alcohol ether, polyglyceryl fatty acid ester,
Polysiloxanes, polyether modified siloxane.
A kind of metal nano conductive ink preparation method, comprise the following steps：
1st, a certain amount of macromolecule resin or the stirring of its mixture are added aforementioned high boiling solvent or its mixture, be heated to
60-120 DEG C of dissolving 30-120min, prepares the high-molecular resin solution of 0-5wt%, referred to as component A；
2nd, methyl alcohol, ethanol, butane, hexane, hexamethylene etc. can will be dissolved in less than the metallorganics of 150 DEG C of decomposition by low temperature
In low boiling point solvent, referred to as component B；
3rd, by gold, silver in the range of 1-500nm for the particle diameter, copper nano-particle powder, it is proportionally added into component A cooling down
In, it is then mixed into component B of certain volume；
4th, by above-mentioned steps 3) mixture that obtains passes through grindings, high speed shear, three roller banburyings promote to disperse, and obtain sticky
Component C；
5th, aforementioned high boiling solvent or its mixture or component A are added in component C by a certain percentage, adjustment system is glued
Degree, metal nanoparticle content, obtain final metal nano conductive ink.
Above-mentioned macromolecule resin is ethyl cellulose, hydroxypropyl cellulose, acrylic resin, polyurethane resin；Above-mentioned
Metallorganic, there is following structure M-X1-R-X2, wherein：M is gold, silver, copper ion, and R is alkyl chain, and usual R contains 1-4
Individual carbon atom, X1 is the functional group connecting metal ion, and X2 is the functional group dispersibling gold, silver, copper nano-particle；Above-mentioned
High boiling solvent be glycol propyl ether, butyl glycol ether, diethylene glycol ether, diethylene glycol propyl ether, butyl, third
Glycol propyl ether, propandiol butyl ether, dipropylene glycol ethyl ether, dipropylene glycol propyl ether, dipropylene, glycol propyl ether acetate,
2-Butoxyethyl acetate, diethylene glycol ether acetate, diethylene glycol propyl ether acetate, butyl acetate, third
Glycol propyl ether acetate, propandiol butyl ether acetate, dipropylene glycol ethyl ether acetate, dipropylene glycol propyl ether acetate, dipropyl two
Alcohol monobutyl ether acetate, ethylene glycol, terpinol, petroleum ether.
Due to technique scheme, the beneficial effects of the present invention is：Realize the stable dispersion of metal nanoparticle, and
Low temperature decomposes, at being less than 150 DEG C, the fusion improving metal nanoparticle, thus realizing low-temperature sintering, high connductivity and big thickness print
Brush, and be widely used in various metal nano conductive inks and preparation method thereof.
Specific embodiment
With specific embodiment, the present invention is further illustrated below：
Embodiment 1：
1) ethyl cellulose is stirred and add dipropylene, be heated to 60-80 DEG C of dissolving 60-120min, make dense
The high-molecular resin solution of degree 0-50g/L, referred to as component A；
2) by can the metallorganic AgOOC-CH2OCH2CH2OCH2CH2OH of low-temperature decomposition to be dissolved in ethanol low boiling molten
In agent, obtain concentration 10-40wt%, referred to as component B；
3) the nano silver particles powder (in the range of particle diameter 50-150nm) obtaining polyol process synthesis adds in A, stirring system
Become concentration 80wt% dispersion liquid, be then proportionally added into component B；
4) by step 3) mixture that obtains passes through to grind and promotes dispersion, obtains sticky component C；
5) terpinol is added in component C by a certain percentage, adjustment system viscosity, metal nanoparticle content, obtains
Silver nanoparticle conductive ink.
The silver nanoparticle conductive ink obtaining in embodiment 1 is tested with general business type R2R gravure equipment, achievable 1-
3um thickness, the printing of the thinnest 50um line footpath, less than 150 DEG C of low-temperature sintering resistivity on art paper as little as 5u Ω cm,
As little as 10u Ω cm in PET film.
Embodiment 2:
1) acrylate is stirred and add aforementioned alcohol ether and alcohol ester mixed solvent, be heated to 80-100 DEG C of dissolving 60-
120min, makes the high-molecular resin solution of concentration 0-50g/L, referred to as component A；
2) the metallorganic AgOOC-CH2OCH2CH2NHCH2CH2NH2 of low-temperature decomposition methyl alcohol low boiling can will be dissolved in
In solvent, obtain concentration 10-40wt%, referred to as component B；
3) nanometer copper particle powder (particle diameter 200-500nm) is added in A, stirring makes concentration 80wt% dispersion liquid, then
It is proportionally added into component B；
4) by step 3) mixture that obtains promotes dispersion by high speed shear, obtains sticky component C；
5) terpinol is added in component C by a certain percentage, adjustment system viscosity, metal nanoparticle content, obtains
Copper nanometer conductive ink.
The copper nanometer conductive ink obtaining in embodiment 2 is tested with general business type R2R gravure equipment, achievable 1-
3um thickness, the printing of the thinnest 50um line footpath, less than 150 DEG C of low-temperature sintering resistivity on art paper as little as 10u Ω .cm,
As little as 20u Ω .cm in PET film.
Embodiment 3:
1) by can the metallorganic AgSCH2CH2OCH2CH2OCH2CH2OH of low-temperature decomposition to be dissolved in ethanol low boiling molten
In agent, obtain concentration 10-40wt%, referred to as component A；
2) nano silver particles powder (in the range of particle diameter 10-50nm) is added aforementioned alcohol ether and alcohol ester mixed solvent, make dense
Degree 80wt% dispersion liquid, is then proportionally added into component A；
3) by step 2) mixture that obtains passes through three roller banburyings and promotes dispersion, obtains sticky component B；
4) mixed solvents such as terpinol are added in component B by a certain percentage, adjustment system viscosity, metal nanoparticle
Content, obtains silver nanoparticle conductive ink.
The silver nanoparticle conductive ink obtaining in embodiment 3 is adopted Dimatix DMP-2831 equipment inkjet printing to test,
Achievable 0.5-1um thickness, the printing of the thinnest 50um line footpath, less than 150 DEG C of low-temperature sintering resistivity on art paper as little as 5u
Ω .cm, as little as 10u Ω .cm in PET film.
Embodiment 4:
1) will be able to the metallorganic AgSCH2CH2NHCH2CH2N2 of low-temperature decomposition be dissolved in ethanol low boiling point solvent,
Obtain concentration 10-40wt%, referred to as component A；
2) nano Au particle powder (in the range of particle diameter 5-20nm) is added aforementioned alcohol ether and alcohol ester mixed solvent, make concentration
80wt% dispersion liquid, is then proportionally added into component A；
3) by step 2) mixture that obtains passes through to grind and promotes dispersion, obtains sticky component B；
4) mixed solvents such as terpinol are added in component B by a certain percentage, adjustment system viscosity, metal nanoparticle
Content, obtains gold nano conductive ink.
The gold nano conductive ink obtaining in embodiment 4 is adopted Dimatix DMP-2831 equipment inkjet printing to test,
Achievable 0.5-1um thickness, the printing of the thinnest 50um line footpath, less than 200 DEG C of low-temperature sintering resistivity on art paper as little as 5u
Ω .cm, as little as 10u Ω .cm in PET film.
Claims (10)
1. a kind of metal nano conductive ink, its group is divided into：
1) gold, silver in the range of 1-500nm for the particle diameter, copper nano-particle powder, content 10-60wt%；
2) 150 DEG C of metallorganics decomposing, content 5-20wt% can be less than by low temperature；
3) non-volatile organic principle, consumption 0-1wt%；
4) volatilize organic principle, consumption 20-80wt%.
2. a kind of metal nano conductive ink according to claim 1 it is characterised in that：Described metallorganic, tool
There is following structure：M-X1-R-X2,
Wherein：M is gold, silver, copper ion；R is alkyl chain, and usual R contains 1-4 carbon atom；X1 is the sense connecting metal ion
Group；X2 is the functional group dispersibling gold, silver, copper nano-particle.
3. a kind of metal nano conductive ink according to claim 1 it is characterised in that：Described non-volatile organic principle
For macromolecule resin, described macromolecule resin is ethyl cellulose, hydroxypropyl cellulose, acrylic resin, polyurethane resin.
4. a kind of metal nano conductive ink according to claim 1 it is characterised in that：Described volatilization organic principle is
High boiling solvent or surface modifier.
5. a kind of metal nano conductive ink according to claim 4 it is characterised in that：Described high boiling solvent is second
Glycol propyl ether, butyl glycol ether, diethylene glycol ether, diethylene glycol propyl ether, butyl, propylene glycol propyl ether, propane diols
Butyl ether, dipropylene glycol ethyl ether, dipropylene glycol propyl ether, dipropylene, glycol propyl ether acetate, butyl glycol ether acetic acid
Ester, diethylene glycol ether acetate, diethylene glycol propyl ether acetate, butyl acetate, propylene glycol propyl ether acetate,
Propandiol butyl ether acetate, dipropylene glycol ethyl ether acetate, dipropylene glycol propyl ether acetate, dipropylene acetate, second
Glycol, terpinol, petroleum ether.
6. a kind of metal nano conductive ink according to claim 4 it is characterised in that：Described surface modifier is organic
Amine, organic carboxyl acid, polyethylene oxide and polyoxy propane copolymer, sorbitan fatty acid ester, sucrose fatty ester, polyoxyethylene
Fatty alcohol ether, poly-for polyoxyethylene fatty alcohol ether, polyglyceryl fatty acid ester, polysiloxanes, polyether modified siloxane.
7. a kind of preparation method of metal nano conductive ink, comprises the following steps：
1) macromolecule resin or the stirring of its mixture are added high boiling solvent or its mixture, be heated to 60-120 DEG C of dissolving
30-120min, prepares the high-molecular resin solution of 0-5wt%, referred to as component A；
2) methyl alcohol, ethanol, butane, hexane, hexamethylene low boiling can will be dissolved in less than the metallorganics of 150 DEG C of decomposition by low temperature
In solvent, referred to as component B；
3) by gold, silver in the range of 1-500nm for the particle diameter, copper nano-particle powder, it is added in component A of cooling, then mixes
Enter described component B；
4) by above-mentioned steps 3) mixture that obtains passes through grindings, high speed shear, three roller banburyings promote to disperse, and obtain sticky group
Divide C；
5) high boiling solvent or its mixture or component A are added in component C by a certain percentage, adjustment system viscosity, metal
Nanoparticle content, obtains final metal nano conductive ink.
8. a kind of metal nano conductive ink according to claim 7 preparation method it is characterised in that：Described macromolecule
Resin is ethyl cellulose, hydroxypropyl cellulose, acrylic resin, polyurethane resin.
9. a kind of metal nano conductive ink according to claim 7 preparation method it is characterised in that：Described metal
Organic matter, has following structure M-X1-R-X2, wherein：M is gold, silver, copper ion, and R is alkyl chain, and it is former that usual R contains 1-4 carbon
Son, X1 is the functional group connecting metal ion, and X2 is the functional group dispersibling gold, silver, copper nano-particle.
10. a kind of metal nano conductive ink according to claim 7 preparation method it is characterised in that：Described height
Boiling point solvent is glycol propyl ether, butyl glycol ether, diethylene glycol ether, diethylene glycol propyl ether, butyl, propane diols
Propyl ether, propandiol butyl ether, dipropylene glycol ethyl ether, dipropylene glycol propyl ether, dipropylene, glycol propyl ether acetate, second two
Alcohol monobutyl ether acetate, diethylene glycol ether acetate, diethylene glycol propyl ether acetate, butyl acetate, propane diols
Propyl ether acetate, propandiol butyl ether acetate, dipropylene glycol ethyl ether acetate, dipropylene glycol propyl ether acetate, DPG fourth
Ether acetate, ethylene glycol, terpinol, petroleum ether.
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| CN106398398B CN106398398B (en) | 2020-01-21 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108652753A (en) * | 2018-02-02 | 2018-10-16 | 浙江清华柔性电子技术研究院 | It is used to form the pattern material and labeling method of organism surface label |
| CN110922895A (en) * | 2019-12-16 | 2020-03-27 | 广东南海启明光大科技有限公司 | Preparation process of conductive chemical coating liquid and preparation method of electric conductor |
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| CN104341860A (en) * | 2013-08-01 | 2015-02-11 | 索尼公司 | Nanometer conductive ink and preparing method thereof |
| CN104419261A (en) * | 2013-09-02 | 2015-03-18 | 北京中科纳通电子技术有限公司 | Colorized conductive ink |
| CN105670390A (en) * | 2008-01-30 | 2016-06-15 | 巴斯夫欧洲公司 | Conductive inks |
| CN105670384A (en) * | 2016-03-31 | 2016-06-15 | 广东南海启明光大科技有限公司 | Nano silver gravure ink and preparation method thereof |
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Patent Citations (5)
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| CN101010388A (en) * | 2005-03-04 | 2007-08-01 | 韩商英泰股份有限公司 | Conductive inks and manufacturing method thereof |
| CN105670390A (en) * | 2008-01-30 | 2016-06-15 | 巴斯夫欧洲公司 | Conductive inks |
| CN104341860A (en) * | 2013-08-01 | 2015-02-11 | 索尼公司 | Nanometer conductive ink and preparing method thereof |
| CN104419261A (en) * | 2013-09-02 | 2015-03-18 | 北京中科纳通电子技术有限公司 | Colorized conductive ink |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108652753A (en) * | 2018-02-02 | 2018-10-16 | 浙江清华柔性电子技术研究院 | It is used to form the pattern material and labeling method of organism surface label |
| CN110922895A (en) * | 2019-12-16 | 2020-03-27 | 广东南海启明光大科技有限公司 | Preparation process of conductive chemical coating liquid and preparation method of electric conductor |
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| CN106398398B (en) | 2020-01-21 |
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