CN115650767B - Silver spraying heat treatment color-changing method for mica sheet - Google Patents
Silver spraying heat treatment color-changing method for mica sheet Download PDFInfo
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- CN115650767B CN115650767B CN202211207199.6A CN202211207199A CN115650767B CN 115650767 B CN115650767 B CN 115650767B CN 202211207199 A CN202211207199 A CN 202211207199A CN 115650767 B CN115650767 B CN 115650767B
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 155
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 155
- 239000004332 silver Substances 0.000 title claims abstract description 155
- 238000010438 heat treatment Methods 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 28
- 238000005507 spraying Methods 0.000 title claims abstract description 18
- 241001251094 Formica Species 0.000 title description 8
- 239000010445 mica Substances 0.000 claims abstract description 215
- 229910052618 mica group Inorganic materials 0.000 claims abstract description 215
- 238000007639 printing Methods 0.000 claims abstract description 45
- 239000002994 raw material Substances 0.000 claims abstract description 19
- 238000005245 sintering Methods 0.000 claims abstract description 18
- 238000009835 boiling Methods 0.000 claims abstract description 13
- 238000010304 firing Methods 0.000 claims abstract description 7
- 238000009966 trimming Methods 0.000 claims abstract description 7
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 52
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 51
- ZXSQEZNORDWBGZ-UHFFFAOYSA-N 1,3-dihydropyrrolo[2,3-b]pyridin-2-one Chemical compound C1=CN=C2NC(=O)CC2=C1 ZXSQEZNORDWBGZ-UHFFFAOYSA-N 0.000 claims description 46
- 229910001958 silver carbonate Inorganic materials 0.000 claims description 46
- LKZMBDSASOBTPN-UHFFFAOYSA-L silver carbonate Substances [Ag].[O-]C([O-])=O LKZMBDSASOBTPN-UHFFFAOYSA-L 0.000 claims description 46
- 238000001035 drying Methods 0.000 claims description 33
- 239000000843 powder Substances 0.000 claims description 31
- 238000003756 stirring Methods 0.000 claims description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 29
- 229910052751 metal Inorganic materials 0.000 claims description 29
- 239000002184 metal Substances 0.000 claims description 29
- 239000012153 distilled water Substances 0.000 claims description 28
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 claims description 26
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 26
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 claims description 26
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 26
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 claims description 26
- 239000000853 adhesive Substances 0.000 claims description 24
- 230000001070 adhesive effect Effects 0.000 claims description 22
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 22
- 238000005406 washing Methods 0.000 claims description 20
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical compound CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 claims description 19
- 238000002360 preparation method Methods 0.000 claims description 19
- 238000005303 weighing Methods 0.000 claims description 18
- 239000001856 Ethyl cellulose Substances 0.000 claims description 16
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 claims description 16
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 claims description 16
- 229920001249 ethyl cellulose Polymers 0.000 claims description 16
- 235000019325 ethyl cellulose Nutrition 0.000 claims description 16
- 238000004080 punching Methods 0.000 claims description 16
- 229940116411 terpineol Drugs 0.000 claims description 16
- 238000012360 testing method Methods 0.000 claims description 16
- LZDKZFUFMNSQCJ-UHFFFAOYSA-N 1,2-diethoxyethane Chemical compound CCOCCOCC LZDKZFUFMNSQCJ-UHFFFAOYSA-N 0.000 claims description 15
- 238000001914 filtration Methods 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 15
- ZPPSOOVFTBGHBI-UHFFFAOYSA-N lead(2+);oxido(oxo)borane Chemical compound [Pb+2].[O-]B=O.[O-]B=O ZPPSOOVFTBGHBI-UHFFFAOYSA-N 0.000 claims description 14
- 229910000416 bismuth oxide Inorganic materials 0.000 claims description 13
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 claims description 13
- 238000001764 infiltration Methods 0.000 claims description 12
- 230000008595 infiltration Effects 0.000 claims description 12
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 11
- 239000004677 Nylon Substances 0.000 claims description 10
- 229920004933 Terylene® Polymers 0.000 claims description 10
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 10
- 239000000919 ceramic Substances 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 10
- 238000005485 electric heating Methods 0.000 claims description 10
- 238000000227 grinding Methods 0.000 claims description 10
- 229920001778 nylon Polymers 0.000 claims description 10
- KJFMBFZCATUALV-UHFFFAOYSA-N phenolphthalein Chemical compound C1=CC(O)=CC=C1C1(C=2C=CC(O)=CC=2)C2=CC=CC=C2C(=O)O1 KJFMBFZCATUALV-UHFFFAOYSA-N 0.000 claims description 10
- 239000005020 polyethylene terephthalate Substances 0.000 claims description 10
- 229910052573 porcelain Inorganic materials 0.000 claims description 10
- 238000003892 spreading Methods 0.000 claims description 10
- 230000007480 spreading Effects 0.000 claims description 10
- 235000019441 ethanol Nutrition 0.000 claims description 8
- 239000012535 impurity Substances 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 7
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- 229910001220 stainless steel Inorganic materials 0.000 claims description 6
- 239000010935 stainless steel Substances 0.000 claims description 6
- 229910000831 Steel Inorganic materials 0.000 claims description 5
- 238000000498 ball milling Methods 0.000 claims description 5
- 238000005520 cutting process Methods 0.000 claims description 5
- 210000003298 dental enamel Anatomy 0.000 claims description 5
- 239000000428 dust Substances 0.000 claims description 5
- 238000011010 flushing procedure Methods 0.000 claims description 5
- 238000009766 low-temperature sintering Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 238000003825 pressing Methods 0.000 claims description 5
- 239000000376 reactant Substances 0.000 claims description 5
- 238000007790 scraping Methods 0.000 claims description 5
- 238000007650 screen-printing Methods 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims description 5
- 239000010959 steel Substances 0.000 claims description 5
- 238000003860 storage Methods 0.000 claims description 5
- 239000011230 binding agent Substances 0.000 claims description 2
- 238000009423 ventilation Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- 230000008859 change Effects 0.000 abstract description 4
- 239000011248 coating agent Substances 0.000 abstract description 4
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- 238000002310 reflectometry Methods 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
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- 239000003085 diluting agent Substances 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 239000003995 emulsifying agent Substances 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 238000005461 lubrication Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- -1 oxygen ion Chemical class 0.000 description 2
- 230000008719 thickening Effects 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
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- 238000005282 brightening Methods 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a mica sheet silver-spraying heat treatment color-changing method, which comprises the following steps of: selecting and stripping mica sheets: selecting and trimming mica slabs, peeling the selected thick mica slabs by using a peeling knife, and grading the peeled mica slabs according to thickness; classifying the thickness of mica sheets: classifying the thickness of the flake mica in the step by using a dial indicator, wherein the allowable error of each specification is +/-1 mu m; firing mica sheets: heating the horse boiling furnace to 570+ -10deg.C, and keeping the temperature, and making mica sheet with size of 14X14 and thickness of 26-30 μm. The invention adopts green pollution-free raw materials when preparing the silver paste, has low production cost, can process the transparent mica sheet into the silver mica sheet after coating the silver paste on the mica sheet by silver printing and sintering, and can be widely applied to toys after color change, so that the mica sheet has high bending resistance and high light reflection, and meets the large-scale production requirement of color change production of the mica sheet.
Description
Technical Field
The invention relates to the technical field of mica sheet color change processing, in particular to a silver spraying heat treatment color change method for mica sheets.
Background
Mica is a rock-making mineral, presents a hexagonal lamellar crystal form, and is one of the main rock-making minerals. The mica crystal has a lamellar structure, is in a flaky crystal, mainly takes a hexagonal flaky crystal, has very high insulation and heat insulation performance and good chemical stability, has strong acid, alkali and pressure resistance, is an important raw material for manufacturing electrical equipment, and has double refraction capability, so that the mica is also an optical instrument material for manufacturing a polarizing plate.
Meanwhile, mica is also one of nonmetallic minerals widely used in modern industry and civil production, and mica paillette is an application form of mica. From the appearance color, mica has more than ten colors, and the main colors are as follows: white, black, gold, golden red, light green, dark green, light red, dark red, sky-gold, sky-yellow, and the like. The mica for the paillette is prepared by raw ore, crushing, dehumidifying, impurity removing, screening, weighing and bagging, and mainly adopts the physical color of the mica.
The existing mica paillette is generally applied in the following aspects: the inner and outer walls of the building are sprayed, most of the paint can be used in real stone paint filler, and the paint can be independently sprayed, so that the building surface can be sparkling, beautiful, noble and elegant; the organic glass products are properly filled with the mono-color or mixed-color mica paillettes, so that the ornamental value of the organic glass products can be greatly increased, and the aesthetic feeling is improved; the plastic product is added with a certain amount of mica paillettes, so that monotonous feeling can be removed, and appreciation can be improved; the application of the mica paillette in decoration and appreciation is realized by the characteristics of the mica paillette.
However, when the mica sheet is used for decoration, the existing mica paillette cannot meet the requirements of people on illumination colors, and the color is single, because the existing mica sheets are mostly transparent after being processed, the mica sheets cannot be applied to paillettes of various electronic toys and ornaments such as light reflection and the like.
For this purpose, a silver-spraying heat treatment color-changing method for mica sheets is provided.
Disclosure of Invention
The invention mainly aims to provide a silver spraying heat treatment color-changing method for mica sheets, which can effectively solve the problems that the color of the existing mica paillette cannot meet the requirements of people on illumination color, and the color is single, because the existing mica sheets are mostly transparent after being treated, and the mica sheets cannot be applied to paillettes of various electronic toys and ornaments such as reflection.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the silver spraying heat treatment color-changing method for the mica sheet comprises the following steps of:
step one: selecting and stripping mica sheets: selecting and trimming mica slabs, peeling the selected thick mica slabs by using a peeling knife, and grading the peeled mica slabs according to thickness;
Step two: classifying the thickness of mica sheets: classifying the thickness of the flake mica in the step by using a dial indicator, wherein the allowable error of each specification is +/-1 mu m;
step three: firing mica flakes by binding Kong Pei: punching the mica sheet by adopting a puncture needle, wherein 10-20 holes are punched in the unit/cm 2, and punching Kong Zhishi is performed on a plurality of single sheets on the mica sheet without punching the whole mica sheet; heating a horse boiling furnace to 570+/-10 ℃ and keeping the temperature, lightly assisting a mica sheet with the size specification of 14X14 and the thickness specification of 26-30 mu m in a metal net tray, uniformly placing the mica sheet in the furnace, closing a furnace door and baking for 3-8 minutes, clamping the metal net tray out by using a long-handle forceps clamp, placing the metal net tray on an operating platform, and lightly clamping the metal net tray in a container by using forceps;
step four: cleaning: placing the mica sheet baked in the steps in boiling distilled water, adding 1% ammonia water for rinsing, shaking a mesh screen during rinsing, rinsing for several times by using distilled water, taking out after water drops are dried, and placing the mica sheet in a copper wire mesh disc; placing the cleaned mica sheet into a baking oven with the temperature of 160+/-20 ℃ for drying until the mica sheet is completely dried, and taking out;
step five: preparing silver paste: preparing silver paste for printing, and weighing the following raw materials in parts by weight: 1400-1600 parts of silver mud, 500-700 parts of adhesive, 100-300 parts of terpineol, 30.5-32.5 parts of bismuth oxide, 20-28 parts of lead borate and 80-120 parts of ethylene glycol monoethyl ether;
step six: preparing a screen:
s11, spreading the terylene film on an insulating plate, and engraving the required silver-coated size on the insulating plate by using a blade and a steel plate ruler, wherein the inner frame size of the screen printing frame is (12+/-0.3) X (12+/-0.3), and the outer frame size is 14X14;
S12, fastening a nylon screen on the frame, and tightly attaching the pre-carved terylene film on the nylon screen by using silver paste;
Step seven: silver printing:
s21, adding qualified silver paste sieved by a 170-180-mesh sieve into a enamel tray by using a spoon, and adjusting the concentration of the silver paste by using ethylene glycol diethyl ether so as to be suitable for printing;
S22, turning on a power switch, and adjusting a pressure regulator of the electric heating plate until the temperature of the baking sheet plate is 90-100 ℃;
s23, neatly and lightly placing the mica sheets into a printing hopper, and carrying out small placement each time to avoid damaging the mica sheets;
S24, sucking the mica sheet on a workbench, enabling a vacuum rubber brush to be stuck with a proper amount of silver paste, pressing down a frame stuck with a printing screen, and uniformly scraping the frame on a screen by flat lifting;
s25, sucking the printed films on a film drying plate on an electric heating film, drying the films, pouring the films into a film storage disc, printing the reverse side after all the films in a hopper are printed, paying attention to the fact that two silver layers are overlapped when the reverse side is printed, and printing the two silver layers of each batch of films by using a template;
step eight: sintering and infiltrating:
S31, checking whether the furnace temperature reaches the prescribed 280-300 ℃;
S32, scattering the rectangular sheets subjected to double-sided printing on a metal net disc, and putting the rectangular sheets into a infiltration furnace for infiltration, wherein the first time of low temperature is 300 ℃, and the sintering is carried out for 10 minutes;
S33, after the low-temperature sintering, checking and separating according to different types and thicknesses, performing sintering permeation at the high temperature of 570+/-10 ℃ for 2-3 minutes on qualified mica sheets after checking and separating, and then dragging the mica sheets to a furnace mouth for 2 minutes and taking out;
Step nine: slicing: cutting off the non-discolored part in the step, namely subtracting the inner frame size (12+/-0.3) X (12+/-0.3) part of the screen frame from the size specification 14X14, so that the final finished product is the discolored mica sheet.
Further, in the first step, the size specification classification of the mica sheet is as follows: 7X14, 12X12, 14X14, 16X16, 10X20, 19X25, 25X25, 20X30, 13X29, 17X34, 20X34, 30X40, 40X50; in the second step, the thickness grading of the mica sheet is as follows: the first gear is 14-16 μm, the second gear is 17-19 μm, the third gear is 20-22 μm, the fourth gear is 22-24 μm, the fifth gear is 26-30 μm, the sixth gear is 31-35 μm, the seventh gear is 36-40 μm, and the eighth gear is 41-45 μm.
Further, the invention also provides a silver paste preparation method which specifically comprises the following steps:
s41, preparing silver paste for printing, wherein the raw materials are weighed according to the following components:
1400-1600 parts of silver mud,
The adhesive agent 500-700 is used as a binder,
100-300 Parts of terpineol,
30.5 To 32.5 percent of bismuth oxide,
20-28 Parts of lead borate,
80-120 Parts of ethylene glycol diethyl ether;
S42, putting silver paste raw materials to be prepared into a porcelain bottle;
s43, tightly covering and sealing, and then placing the ceramic balls on a ball mill for operation, wherein the ceramic balls are prevented from being broken during operation;
s44, controlling the ball milling time to be 100+/-10 hours, and controlling the running speed of the ball mill to be 75+/-5 rpm;
S45, filtering the sample test piece with a 170-180 mesh sieve after the sample test piece is normal, and storing the sample test piece in a clean and light-proof environment for later use;
The silver mud comprises the following components in percentage by weight: silver carbonate 850-1050, rosin 4.5-5.0, collodion 3-8, n-butanol 1750-1850 and triethanolamine 75-80; wherein, the silver carbonate component and the weight percentage content are: 10-15 parts of silver nitrate, 50-60 parts of ethanol, 4-8 parts of rosin, 30-50 parts of sodium carbonate and 150-200 parts of distilled water;
the adhesive comprises the following components in percentage by weight: terpineol 250-270, ethyl cellulose 35-50, ethylene glycol diethyl ether 460-470.
Further, the invention also provides a preparation method of the silver mud, which specifically comprises the following steps:
S51, weighing 950-1000g of silver carbonate powder, pouring the silver carbonate powder into a stainless steel pot, pouring 1700-1800me of n-butanol, heating and stirring;
S52, when the temperature is raised to 80-90 ℃, pouring 4-5g of rosin powder and 4.5-6.5g of collodion, and continuously stirring;
S53, dropwise adding 78-79g of n-butanol and 78-79g of triethanolamine by using a separating funnel when the temperature reaches 90-95 ℃, stopping heating, keeping the temperature at 93+/-1 ℃ for 2-3 hours, and keeping the temperature for 45-50 minutes, wherein the temperature is still 93+/-1 ℃;
s54, taking out silver mud, cooling for 10-12 hours, washing with absolute ethyl alcohol for 5-6 times, removing impurities, then placing in a ventilation opening, naturally drying, and grinding and storing the dried silver mud;
s55, placing the crushed silver mud in a place which is dry, light-proof and clean to prevent dust.
Further, the invention also provides a preparation method of the silver carbonate, which specifically comprises the following steps:
S61, weighing 5-7g of rosin, grinding into powder, adding 50-58g of 99.5% ethanol, and dissolving into yellowish brown liquid, namely 9% rosin water;
s62, adding 150-170me of distilled water into 35-45g of sodium carbonate, heating to fully dissolve the sodium carbonate into colorless transparent sodium carbonate solution, and cooling for later use;
S63, adding 250-300me of distilled water into 100-140g of silver nitrate, stirring for 15-20 minutes, pouring 10-14me of rosin water, and continuously stirring for a plurality of minutes, wherein the rotating speed of a stirrer is 160-180 revolutions per minute;
s64, gradually dripping the sodium carbonate solution into the silver nitrate solution by using a separating funnel, stopping adding the sodium carbonate solution when the reactant is alkaline after dripping the 1% phenolphthalein solution into pink after finishing dripping for 2-3 hours, and continuously stirring for a plurality of minutes;
S65, spreading filter paper in a porcelain funnel, pouring the prepared silver carbonate solution for filtering, flushing with distilled water and suction-filtering until the washing liquid is not alkaline, and dripping the washing liquid which is not red from the 1% phenolphthalein solution into the discharged washing water;
S66, placing the washed silver carbonate powder in an oven at 55-60 ℃ for drying for 5-7 days until no water exists, so that the silver carbonate is light yellow powder.
Further, the invention also provides a preparation method of the adhesive, which comprises the steps of weighing 250-270g of terpineol, 40-45g of ethyl cellulose and 450-470g of ethylene glycol diethyl ether, mixing and stirring until the ethyl cellulose is completely dissolved.
Further, removing the mica sheets with low utilization rate such as green, black, spots, impurities, bubbles and unevenness, which account for more than 5% of the total area of the mica sheets, and removing serious burrs, cracks and uneven parts at the edges of the mica sheets when the mica sheets are selected in the first step; when the mica sheet is peeled, uneven thickness and cracks of the mica edge are removed, and if bubbles are found, a puncture needle is used for puncturing a small hole.
Compared with the prior art, the invention has the following beneficial effects:
According to the invention, the self-made silver carbonate can effectively improve the silver content, so that the silver content of the silver carbonate is kept at 74% -78%, wherein 99.5% ethanol and rosin are adopted in the preparation of the silver carbonate, so that the effects of preventing oxidization and improving the brightness of the silver carbonate can be effectively achieved; when preparing silver mud, the collodion can effectively improve the toughness of the silver mud, the added triethanolamine can play a role of an emulsifier to realize thickening and maintain PH balance, an alkaline environment is provided to promote the hydrolysis of silver carbonate, the coating effect is good, meanwhile, the characteristics of fineness and brightness of the silver mud paste are effectively improved, the added n-butanol can be used as a solvent for preparing the silver mud so as to improve the reaction efficiency of the silver carbonate, rosin, collodion and triethanolamine, and the silver content in the silver mud prepared by adopting the raw materials can be effectively ensured to be maintained above 80%; the special adhesive applied to the silver paste is prepared, and the added ethyl cellulose is used as an organic carrier, so that the lubrication degree of the silver paste in use can be improved, wherein the added ethylene glycol diethyl ether is used as a diluent solvent, so that the dissolution of terpineol and ethyl cellulose can be effectively ensured; when preparing silver paste, the added silver paste is prepared from silver carbonate prepared by the method, so that the silver content can be effectively ensured, meanwhile, the added adhesive can improve the lubricity of the silver paste when in use, the added bismuth oxide has extremely high oxygen ion conductivity, and the added lead borate has a drying effect as a drier;
When the silver paste is coated on the surface of the mica sheet, the quick evaporation of the solvent can be realized under the action of the collodion so as to form a layer of film on the surface of the mica sheet;
The prepared adhesive is added, so that the adhesive force is improved, the silver paste and the mica sheet are easier to be eutectic-melted during sintering and infiltration, a new uniform phase is formed, the adhesive force of a silver layer is enhanced, the mica sheet after hole punching is more convenient for the combination of the mica sheet and silver mud, and the color-changing effect of the mica sheet is effectively improved;
The silver paste is prepared from green pollution-free raw materials, the production cost is low, after silver paste is coated on the mica sheet and silver printing and baking are carried out, the transparent mica sheet can be processed into silver mica sheets, and the color-changed mica sheets can be widely applied to toys, so that the mica sheets have high bending resistance and high reflectivity, and meet the large-scale production requirements of color-changing production of the mica sheets.
Drawings
Fig. 1 is a flow chart of a method for changing color of mica sheets by silver spraying heat treatment.
Fig. 2 is a diagram of an original, non-color-change treated mica sheet.
Fig. 3 is a diagram of a mica sheet subjected to a discoloration method by a silver spray heat treatment.
Detailed Description
The invention is further described in connection with the following detailed description, in order to make the technical means, the creation characteristics, the achievement of the purpose and the effect of the invention easy to understand.
Example 1. As shown in fig. 1, the silver spraying heat treatment color-changing method for mica sheets comprises the following steps:
step one: selecting and stripping mica sheets: selecting and trimming mica slabs, peeling the selected thick mica slabs by using a peeling knife, and grading the peeled mica slabs according to thickness;
Step two: classifying the thickness of mica sheets: classifying the thickness of the flake mica in the step by using a dial indicator, wherein the allowable error of each specification is +/-1 mu m;
Step three: firing mica flakes by binding Kong Pei: punching the mica sheet by adopting a puncture needle, wherein 10-20 holes are punched in the unit/cm 2, and punching Kong Zhishi is performed on a plurality of single sheets on the mica sheet without punching the whole mica sheet; heating a horse boiling furnace to 570 ℃ and keeping constant temperature, lightly assisting a mica sheet with the size specification of 14X14 and the thickness specification of 26-30 mu m in a metal net tray, uniformly placing the mica sheet in the furnace, closing a furnace door and baking for 5 minutes, clamping the metal net tray out by using a long-handle forceps clamp, placing the metal net tray on an operation table, and lightly clamping the metal net tray in a container by using forceps;
step four: cleaning: placing the mica sheet baked in the steps in boiling distilled water, adding 1% ammonia water for rinsing, shaking a mesh screen during rinsing, rinsing for several times by using distilled water, taking out after water drops are dried, and placing the mica sheet in a copper wire mesh disc; placing the cleaned mica sheet into a drying oven with the temperature of 160 ℃ for drying until the mica sheet is completely dried, and taking out;
Step five: preparing silver paste:
s41, preparing silver paste for printing, wherein the raw materials are weighed according to the following components:
The silver paste 1400 is formed from a mixture of silver paste,
The adhesive 500 is applied to the substrate by a bonding process,
A terpineol (100) is used,
30.5 Percent of bismuth oxide and the total content of the bismuth oxide,
A lead borate (20) is added to the composition,
Ethylene glycol ethyl ether 80;
S42, putting silver paste raw materials to be prepared into a porcelain bottle;
s43, tightly covering and sealing, and then placing the ceramic balls on a ball mill for operation, wherein the ceramic balls are prevented from being broken during operation;
s44, controlling the ball milling time to be 100 hours, wherein the running speed of the ball mill is 75 rpm;
s45, filtering the sample test piece into a container by using a 170-mesh sieve after the sample test piece is normal, and storing the sample test piece in a clean and light-proof environment for later use;
the preparation method of the silver mud specifically comprises the following steps:
S51, weighing 950g of silver carbonate powder, pouring the silver carbonate powder into a stainless steel pot, pouring 1700me of n-butanol, heating and stirring;
S52, pouring 4g of rosin powder and 4.5g of collodion when the temperature is raised to 80 ℃, and continuously stirring;
s53, when the temperature reaches 90 ℃, 78g of n-butanol and 78g of triethanolamine are dripped by using a separating funnel, the temperature is stopped rising, the temperature is kept at 92 ℃ and is kept for 2 hours, and the heat preservation is continued for 45 minutes, wherein the temperature is still 93 ℃;
S54, taking out silver mud, cooling for 10 hours, washing with absolute ethyl alcohol for 5 times, removing impurities, then placing in a vent, naturally drying, and grinding and storing the dried silver mud;
s55, placing the crushed silver mud in a place which is dry, light-proof and clean to prevent dust;
the preparation method of the silver carbonate specifically comprises the following steps:
S61, weighing 5g of rosin, grinding into powder, adding 50g of ethanol with the concentration of 99.5% and dissolving into a yellowish brown liquid, namely 9% of rosin water;
S62, adding 150me of distilled water into 35g of sodium carbonate, heating to fully dissolve the sodium carbonate into colorless transparent sodium carbonate solution, and cooling for later use;
s63, adding distilled water into 100g of silver nitrate, stirring for 15 minutes, pouring 10me of rosin water, and continuously stirring for several minutes, wherein the rotating speed of a stirrer is 160 revolutions per minute;
s64, gradually dripping the sodium carbonate solution into the silver nitrate solution by using a separating funnel, stopping adding the sodium carbonate solution when the reactant is alkaline after dripping the 1% phenolphthalein solution into pink after finishing dripping for 2 hours, and continuously stirring for a plurality of minutes;
S65, spreading filter paper in a porcelain funnel, pouring the prepared silver carbonate solution for filtering, flushing with distilled water and suction-filtering until the washing liquid is not alkaline, and dripping the washing liquid which is not red from the 1% phenolphthalein solution into the discharged washing water;
s66, placing the washed silver carbonate powder in a 55 ℃ oven for drying for 5 days until no moisture exists, so that the silver carbonate is light yellow powder;
The preparation method of the adhesive comprises the steps of weighing 250g of terpineol, 40g of ethyl cellulose and 450g of ethylene glycol diethyl ether, mixing and stirring until the ethyl cellulose is completely dissolved;
step six: preparing a screen:
s11, spreading the terylene film on an insulating plate, and engraving the required silver-coated size on the insulating plate by using a blade and a steel plate ruler, wherein the inner frame size of the screen printing frame is (12+/-0.3) X (12+/-0.3), and the outer frame size is 14X14;
S12, fastening a nylon screen on the frame, and tightly attaching the pre-carved terylene film on the nylon screen by using silver paste;
Step seven: silver printing:
S21, adding qualified silver paste sieved by a 170-mesh sieve into a enamel tray by using a spoon, and adjusting the concentration of the silver paste by using ethylene glycol monoethyl ether so as to be suitable for printing;
s22, turning on a power switch, and adjusting a pressure regulator of the electric heating plate until the temperature of the baking sheet plate is 90 ℃;
s23, neatly and lightly placing the mica sheets into a printing hopper, and carrying out small placement each time to avoid damaging the mica sheets;
S24, sucking the mica sheet on a workbench, enabling a vacuum rubber brush to be stuck with a proper amount of silver paste, pressing down a frame stuck with a printing screen, and uniformly scraping the frame on a screen by flat lifting;
s25, sucking the printed films on a film drying plate on an electric heating film, drying the films, pouring the films into a film storage disc, printing the reverse side after all the films in a hopper are printed, paying attention to the fact that two silver layers are overlapped when the reverse side is printed, and printing the two silver layers of each batch of films by using a template;
step eight: sintering and infiltrating:
S31, checking whether the furnace temperature reaches a specified 280 ℃;
S32, scattering the rectangular sheets subjected to double-sided printing on a metal net disc, and putting the rectangular sheets into a infiltration furnace for infiltration, wherein the first time of low temperature is 300 ℃, and the sintering is carried out for 10 minutes;
s33, after the low-temperature sintering, checking and separating according to different types and thicknesses, sintering and infiltrating at a high temperature of 570 ℃ for 2 minutes after checking and separating qualified mica sheets, and then dragging the mica sheets to a furnace mouth for 2 minutes and taking out;
Step nine: slicing: cutting off the non-discolored part in the step, namely subtracting the inner frame size (12+/-0.3) X (12+/-0.3) part of the screen frame from the size specification 14X14, so that the final finished product is the discolored mica sheet.
Example 2. As shown in fig. 1, the silver spraying heat treatment color-changing method for mica sheets comprises the following steps:
step one: selecting and stripping mica sheets: selecting and trimming mica slabs, peeling the selected thick mica slabs by using a peeling knife, and grading the peeled mica slabs according to thickness;
Step two: classifying the thickness of mica sheets: classifying the thickness of the flake mica in the step by using a dial indicator, wherein the allowable error of each specification is +/-1 mu m;
Step three: firing mica flakes by binding Kong Pei: punching the mica sheet by adopting a puncture needle, wherein 10-20 holes are punched in the unit/cm 2, and punching Kong Zhishi is performed on a plurality of single sheets on the mica sheet without punching the whole mica sheet; heating a horse boiling furnace to 570 ℃ and keeping constant temperature, lightly assisting a mica sheet with the size specification of 14X14 and the thickness specification of 26-30 mu m in a metal net tray, uniformly placing the mica sheet in the furnace, closing a furnace door and baking for 5 minutes, clamping the metal net tray out by using a long-handle forceps clamp, placing the metal net tray on an operation table, and lightly clamping the metal net tray in a container by using forceps;
step four: cleaning: placing the mica sheet baked in the steps in boiling distilled water, adding 1% ammonia water for rinsing, shaking a mesh screen during rinsing, rinsing for several times by using distilled water, taking out after water drops are dried, and placing the mica sheet in a copper wire mesh disc; placing the cleaned mica sheet into a drying oven with the temperature of 160 ℃ for drying until the mica sheet is completely dried, and taking out;
Step five: preparing silver paste:
s41, preparing silver paste for printing, wherein the raw materials are weighed according to the following components:
The silver paste 1500 is used as a raw material,
The adhesive 600 is applied to the substrate by a bonding process,
Terpineol 200,
31.5 Percent of bismuth oxide and the total content of the bismuth oxide,
The lead borate (24) is provided with a lead borate,
Ethylene glycol diethyl ether 100;
S42, putting silver paste raw materials to be prepared into a porcelain bottle;
s43, tightly covering and sealing, and then placing the ceramic balls on a ball mill for operation, wherein the ceramic balls are prevented from being broken during operation;
s44, controlling the ball milling time to be 100 hours, wherein the running speed of the ball mill is 75 rpm;
s45, filtering the sample test piece into a container by using a 170-mesh sieve after the sample test piece is normal, and storing the sample test piece in a clean and light-proof environment for later use;
the preparation method of the silver mud specifically comprises the following steps:
s51, weighing 975g of silver carbonate powder, pouring the silver carbonate powder into a stainless steel pot, pouring 1750me of n-butanol, heating and stirring;
S52, when the temperature is raised to 80 ℃, 4.5g of rosin powder and 5.5g of collodion are poured in and stirring is continued;
S53, dropwise adding 78.5g of n-butanol and 78.5g of triethanolamine by using a separating funnel when the temperature reaches 90 ℃, stopping heating, keeping the temperature at 93 ℃ for 2 hours, and keeping the temperature for 45 minutes, wherein the temperature is still 93 ℃;
S54, taking out silver mud, cooling for 10 hours, washing with absolute ethyl alcohol for 5 times, removing impurities, then placing in a vent, naturally drying, and grinding and storing the dried silver mud;
s55, placing the crushed silver mud in a place which is dry, light-proof and clean to prevent dust;
the preparation method of the silver carbonate specifically comprises the following steps:
s61, weighing 6g of rosin, grinding into powder, adding 54g of ethanol with the concentration of 99.5% and dissolving into a yellowish brown liquid, namely 9% of rosin water;
s62, adding 160me distilled water into 40g of sodium carbonate, heating to fully dissolve the sodium carbonate into colorless transparent sodium carbonate solution, and cooling for later use;
S63, adding 275me of distilled water into 120g of silver nitrate, stirring for 15 minutes, pouring 12me of rosin water, and continuously stirring for several minutes, wherein the rotating speed of a stirrer is 160 revolutions per minute;
s64, gradually dripping the sodium carbonate solution into the silver nitrate solution by using a separating funnel, stopping adding the sodium carbonate solution when the reactant is alkaline after dripping the 1% phenolphthalein solution into pink after finishing dripping for 2 hours, and continuously stirring for a plurality of minutes;
S65, spreading filter paper in a porcelain funnel, pouring the prepared silver carbonate solution for filtering, flushing with distilled water and suction-filtering until the washing liquid is not alkaline, and dripping the washing liquid which is not red from the 1% phenolphthalein solution into the discharged washing water;
s66, placing the washed silver carbonate powder in a 55 ℃ oven for drying for 5 days until no moisture exists, so that the silver carbonate is light yellow powder;
the preparation method of the adhesive comprises the steps of weighing 260g of terpineol, 42.5g of ethyl cellulose and 460g of ethylene glycol diethyl ether, mixing and stirring until the ethyl cellulose is completely dissolved;
step six: preparing a screen:
s11, spreading the terylene film on an insulating plate, and engraving the required silver-coated size on the insulating plate by using a blade and a steel plate ruler, wherein the inner frame size of the screen printing frame is (12+/-0.3) X (12+/-0.3), and the outer frame size is 14X14;
S12, fastening a nylon screen on the frame, and tightly attaching the pre-carved terylene film on the nylon screen by using silver paste;
Step seven: silver printing:
S21, adding qualified silver paste sieved by a 170-mesh sieve into a enamel tray by using a spoon, and adjusting the concentration of the silver paste by using ethylene glycol monoethyl ether so as to be suitable for printing;
s22, turning on a power switch, and adjusting a pressure regulator of the electric heating plate until the temperature of the baking sheet plate is 90 ℃;
s23, neatly and lightly placing the mica sheets into a printing hopper, and carrying out small placement each time to avoid damaging the mica sheets;
S24, sucking the mica sheet on a workbench, enabling a vacuum rubber brush to be stuck with a proper amount of silver paste, pressing down a frame stuck with a printing screen, and uniformly scraping the frame on a screen by flat lifting;
s25, sucking the printed films on a film drying plate on an electric heating film, drying the films, pouring the films into a film storage disc, printing the reverse side after all the films in a hopper are printed, paying attention to the fact that two silver layers are overlapped when the reverse side is printed, and printing the two silver layers of each batch of films by using a template;
step eight: sintering and infiltrating:
S31, checking whether the furnace temperature reaches a prescribed 290 ℃;
S32, scattering the rectangular sheets subjected to double-sided printing on a metal net disc, and putting the rectangular sheets into a infiltration furnace for infiltration, wherein the first time of low temperature is 300 ℃, and the sintering is carried out for 10 minutes;
S33, after the low-temperature sintering, checking and separating according to different types and thicknesses, sintering and infiltrating at the high temperature of 570 ℃ for 2-3 minutes, and then dragging the mica sheet to a furnace mouth for 2 minutes and taking out;
Step nine: slicing: cutting off the non-discolored part in the step, namely subtracting the inner frame size (12+/-0.3) X (12+/-0.3) part of the screen frame from the size specification 14X14, so that the final finished product is the discolored mica sheet.
Example 3. As shown in fig. 1, the silver spraying heat treatment color-changing method for mica sheets comprises the following steps:
step one: selecting and stripping mica sheets: selecting and trimming mica slabs, peeling the selected thick mica slabs by using a peeling knife, and grading the peeled mica slabs according to thickness;
Step two: classifying the thickness of mica sheets: classifying the thickness of the flake mica in the step by using a dial indicator, wherein the allowable error of each specification is +/-1 mu m;
Step three: firing mica flakes by binding Kong Pei: punching the mica sheet by adopting a puncture needle, wherein 10-20 holes are punched in the unit/cm 2, and punching Kong Zhishi is performed on a plurality of single sheets on the mica sheet without punching the whole mica sheet; heating a horse boiling furnace to 570 ℃ and keeping constant temperature, lightly assisting a mica sheet with the size specification of 14X14 and the thickness specification of 26-30 mu m in a metal net tray, uniformly placing the mica sheet in the furnace, closing a furnace door and baking for 5 minutes, clamping the metal net tray out by using a long-handle forceps clamp, placing the metal net tray on an operation table, and lightly clamping the metal net tray in a container by using forceps;
step four: cleaning: placing the mica sheet baked in the steps in boiling distilled water, adding 1% ammonia water for rinsing, shaking a mesh screen during rinsing, rinsing for several times by using distilled water, taking out after water drops are dried, and placing the mica sheet in a copper wire mesh disc; placing the cleaned mica sheet into a drying oven with the temperature of 160 ℃ for drying until the mica sheet is completely dried, and taking out;
Step five: preparing silver paste:
s41, preparing silver paste for printing, wherein the raw materials are weighed according to the following components:
the silver paste 1600 is deposited on the surface of the substrate,
The adhesive 700 is applied to the substrate by a bonding process,
A terpineol (300) in the form of a salt,
32.5 Percent of bismuth oxide, wherein the bismuth oxide is prepared from bismuth oxide,
The lead borate (28) is provided with a lead borate,
Ethylene glycol diethyl ether 100;
S42, putting silver paste raw materials to be prepared into a porcelain bottle;
s43, tightly covering and sealing, and then placing the ceramic balls on a ball mill for operation, wherein the ceramic balls are prevented from being broken during operation;
s44, controlling the ball milling time to be 100 hours, wherein the running speed of the ball mill is 75 rpm;
s45, filtering the sample test piece into a container by using a 170-mesh sieve after the sample test piece is normal, and storing the sample test piece in a clean and light-proof environment for later use;
the preparation method of the silver mud specifically comprises the following steps:
s51, weighing 1000g of silver carbonate powder, pouring the silver carbonate powder into a stainless steel pot, and pouring 1800me of n-butanol into the stainless steel pot for heating and stirring;
S52, pouring 5g of rosin powder and 6.5g of collodion to continue stirring when the temperature is raised to 80 ℃;
S53, when the temperature reaches 90 ℃, using a separating funnel to drop 79g of n-butanol and 79g of triethanolamine, stopping heating, keeping the temperature at 93 ℃, keeping the temperature for 45 minutes after 2 hours, and keeping the temperature at 93 ℃;
S54, taking out silver mud, cooling for 10 hours, washing with absolute ethyl alcohol for 5 times, removing impurities, then placing in a vent, naturally drying, and grinding and storing the dried silver mud;
s55, placing the crushed silver mud in a place which is dry, light-proof and clean to prevent dust;
the preparation method of the silver carbonate specifically comprises the following steps:
S61, weighing 7g of rosin, grinding into powder, adding 58g of ethanol with the concentration of 99.5% and dissolving into a yellowish brown liquid, namely 9% rosin water;
s62, adding 170me distilled water into 45g of sodium carbonate, heating to fully dissolve the sodium carbonate into colorless transparent sodium carbonate solution, and cooling for later use;
S63, adding 300me of distilled water into 140g of silver nitrate, stirring for 15 minutes, pouring 14me of rosin water, and continuously stirring for a plurality of minutes, wherein the rotating speed of a stirrer is 160 revolutions per minute;
s64, gradually dripping the sodium carbonate solution into the silver nitrate solution by using a separating funnel, stopping adding the sodium carbonate solution when the reactant is alkaline after dripping the 1% phenolphthalein solution into pink after finishing dripping for 2 hours, and continuously stirring for a plurality of minutes;
S65, spreading filter paper in a porcelain funnel, pouring the prepared silver carbonate solution for filtering, flushing with distilled water and suction-filtering until the washing liquid is not alkaline, and dripping the washing liquid which is not red from the 1% phenolphthalein solution into the discharged washing water;
s66, placing the washed silver carbonate powder in a 55 ℃ oven for drying for 5 days until no moisture exists, so that the silver carbonate is light yellow powder;
The preparation method of the adhesive comprises the steps of weighing 270g of terpineol, 45g of ethyl cellulose and 470g of ethylene glycol diethyl ether, mixing and stirring until the ethyl cellulose is completely dissolved;
step six: preparing a screen:
s11, spreading the terylene film on an insulating plate, and engraving the required silver-coated size on the insulating plate by using a blade and a steel plate ruler, wherein the inner frame size of the screen printing frame is (12+/-0.3) X (12+/-0.3), and the outer frame size is 14X14;
S12, fastening a nylon screen on the frame, and tightly attaching the pre-carved terylene film on the nylon screen by using silver paste;
Step seven: silver printing:
S21, adding qualified silver paste sieved by a 170-mesh sieve into a enamel tray by using a spoon, and adjusting the concentration of the silver paste by using ethylene glycol monoethyl ether so as to be suitable for printing;
s22, turning on a power switch, and adjusting a pressure regulator of the electric heating plate until the temperature of the baking sheet plate is 90 ℃;
s23, neatly and lightly placing the mica sheets into a printing hopper, and carrying out small placement each time to avoid damaging the mica sheets;
S24, sucking the mica sheet on a workbench, enabling a vacuum rubber brush to be stuck with a proper amount of silver paste, pressing down a frame stuck with a printing screen, and uniformly scraping the frame on a screen by flat lifting;
s25, sucking the printed films on a film drying plate on an electric heating film, drying the films, pouring the films into a film storage disc, printing the reverse side after all the films in a hopper are printed, paying attention to the fact that two silver layers are overlapped when the reverse side is printed, and printing the two silver layers of each batch of films by using a template;
step eight: sintering and infiltrating:
S31, checking whether the furnace temperature reaches a prescribed 300 ℃;
S32, scattering the rectangular sheets subjected to double-sided printing on a metal net disc, and putting the rectangular sheets into a infiltration furnace for infiltration, wherein the first time of low temperature is 300 ℃, and the sintering is carried out for 10 minutes;
s33, after the low-temperature sintering, checking and separating according to different types and thicknesses, sintering and infiltrating at a high temperature of 570 ℃ for 2 minutes after checking and separating qualified mica sheets, and then dragging the mica sheets to a furnace mouth for 2 minutes and taking out;
Step nine: slicing: cutting off the non-discolored part in the step, namely subtracting the inner frame size (12+/-0.3) X (12+/-0.3) part of the screen frame from the size specification 14X14, so that the final finished product is the discolored mica sheet.
Comparative example 1. The mica sheets which are not subjected to silver spraying heat treatment in the same batch as the above embodiment are selected for baking, cleaning and drying, and the specific operation method is as follows:
step one: selecting and stripping mica sheets: selecting and trimming mica slabs, peeling the selected thick mica slabs by using a peeling knife, and grading the peeled mica slabs according to thickness;
Step two: classifying the thickness of mica sheets: classifying the thickness of the flake mica in the step by using a dial indicator, wherein the allowable error of each specification is +/-1 mu m;
Step three: firing mica sheets: heating a horse boiling furnace to 570 ℃ and keeping constant temperature, lightly assisting a mica sheet with the size specification of 14X14 and the thickness specification of 26-30 mu m in a metal net tray, uniformly placing the mica sheet in the furnace, closing a furnace door and baking for 5 minutes, clamping the metal net tray out by using a long-handle forceps clamp, placing the metal net tray on an operation table, and lightly clamping the metal net tray in a container by using forceps;
step four: cleaning: placing the mica sheet baked in the steps in boiling distilled water, adding 1% ammonia water for rinsing, shaking a mesh screen during rinsing, rinsing for several times by using distilled water, taking out after water drops are dried, and placing the mica sheet in a copper wire mesh disc; placing the cleaned mica sheet into a drying oven with the temperature of 160 ℃ for drying until the mica sheet is completely dried, and taking out;
The four sets of spangle mica sheets obtained in examples 1-3 and comparative example 1 above were each tested for reflectance and transparency, and the specific results are shown in table 1:
TABLE 1
From the tests of examples 1 to 3 and comparative example 1 described above, it is seen that: the mica sheet without silver spraying heat treatment has general toughness, so that when the electronic toy and the ornament are decorated, the electronic toy and the ornament cannot achieve good toughness to meet the requirement of use, the mica sheet is easy to be layered and broken, and meanwhile, the expected use effects of light reflection and bright silver light cannot be achieved when the electronic toy and the ornament are decorated and used because the light reflection rate is lower and the transparency is higher, so that the gorgeous degree is only general; however, by adopting the silver spraying heat treatment color-changing method for the mica sheet, the surface of the existing mica sheet can be subjected to silver coating operation, so that the reflectivity of the existing mica sheet is increased, and the existing mica sheet has the characteristic of no light transmission, therefore, the effects of reflecting light and brightening silver light can be realized when the mica sheet is used for decoration, the technological sense of an electronic toy is improved, meanwhile, the toughness of the mica sheet can be effectively improved, and the problem of layering and crushing when the mica sheet is installed and posted for use is avoided.
According to the invention, the self-made silver carbonate can effectively improve the silver content, so that the silver content of the silver carbonate is kept at 74% -78%, wherein 99.5% ethanol and rosin are adopted in the preparation of the silver carbonate, so that the effects of preventing oxidization and improving the brightness of the silver carbonate can be effectively achieved; when preparing silver mud, the collodion can effectively improve the toughness of the silver mud, the added triethanolamine can play a role of an emulsifier to realize thickening and maintain PH balance, an alkaline environment is provided to promote the hydrolysis of silver carbonate, the coating effect is good, meanwhile, the characteristics of fineness and brightness of the silver mud paste are effectively improved, the added n-butanol can be used as a solvent for preparing the silver mud so as to improve the reaction efficiency of the silver carbonate, rosin, collodion and triethanolamine, and the silver content in the silver mud prepared by adopting the raw materials can be effectively ensured to be maintained above 80%; the special adhesive applied to the silver paste is prepared, and the added ethyl cellulose is used as an organic carrier, so that the lubrication degree of the silver paste in use can be improved, wherein the added ethylene glycol diethyl ether is used as a diluent solvent, so that the dissolution of terpineol and ethyl cellulose can be effectively ensured; when preparing silver paste, the added silver paste is prepared from silver carbonate prepared by the method, so that the silver content can be effectively ensured, meanwhile, the added adhesive can improve the lubricity of the silver paste when in use, the added bismuth oxide has extremely high oxygen ion conductivity, and the added lead borate has a drying effect as a drier;
When the silver paste is coated on the surface of the mica sheet, the quick evaporation of the solvent can be realized under the action of the collodion so as to form a layer of film on the surface of the mica sheet;
The prepared adhesive is added, so that the adhesive force is improved, the silver paste and the mica sheet are easier to be eutectic-melted during sintering and infiltration, a new uniform phase is formed, the adhesive force of a silver layer is enhanced, and the color-changing effect of the mica sheet is effectively improved;
The silver paste is prepared from green pollution-free raw materials, the production cost is low, after silver paste is coated on the mica sheet and silver printing and baking are carried out, the transparent mica sheet can be processed into silver mica sheets, and the color-changed mica sheets can be widely applied to toys, so that the mica sheets have high bending resistance and high reflectivity, and meet the large-scale production requirements of color-changing production of the mica sheets.
The foregoing has shown and described the basic principles and main features of the present invention and the advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (4)
1. The silver spraying heat treatment color-changing method for the mica sheet is characterized by comprising the following steps of: the specific operation method comprises the following steps:
step one: selecting and stripping mica sheets: selecting and trimming mica slabs, peeling the selected thick mica slabs by using a peeling knife, and grading the peeled mica slabs according to the size specification;
Step two: classifying the thickness of mica sheets: classifying the thickness of the flake mica in the step by using a dial indicator, wherein the allowable error of each specification is +/-1 mu m;
step three: firing mica flakes by binding Kong Pei: punching the mica sheet by adopting a puncture needle, wherein 10-20 holes are punched in the unit/cm 2, and punching Kong Zhishi is performed on a plurality of single sheets on the mica sheet without punching the whole mica sheet; heating a horse boiling furnace to 570+/-10 ℃ and keeping the temperature, lightly assisting a mica sheet with the size specification of 14X14 and the thickness specification of 26-30 mu m in a metal net tray, uniformly placing the mica sheet in the furnace, closing a furnace door and baking for 3-8 minutes, clamping the metal net tray out by using a long-handle forceps clamp, placing the metal net tray on an operating platform, and lightly clamping the metal net tray in a container by using forceps;
step four: cleaning: placing the mica sheet baked in the steps in boiling distilled water, adding 1% ammonia water for rinsing, shaking a mesh screen during rinsing, rinsing for several times by using distilled water, taking out after water drops are dried, and placing the mica sheet in a copper wire mesh disc; placing the cleaned mica sheet into a baking oven with the temperature of 160+/-20 ℃ for drying until the mica sheet is completely dried, and taking out;
step five: preparing silver paste: preparing silver paste for printing, and weighing the following raw materials in parts by weight: 1400-1600 parts of silver mud, 500-700 parts of adhesive, 100-300 parts of terpineol, 30.5-32.5 parts of bismuth oxide, 20-28 parts of lead borate and 80-120 parts of ethylene glycol monoethyl ether;
step six: preparing a screen:
s11, spreading the terylene film on an insulating plate, and engraving the required silver-coated size on the insulating plate by using a blade and a steel plate ruler, wherein the inner frame size of the screen printing frame is (12+/-0.3) X (12+/-0.3), and the outer frame size is 14X14;
S12, fastening a nylon screen on the frame, and tightly attaching the pre-carved terylene film on the nylon screen by using silver paste;
Step seven: silver printing:
s21, adding qualified silver paste sieved by a 170-180-mesh sieve into a enamel tray by using a spoon, and adjusting the concentration of the silver paste by using ethylene glycol diethyl ether so as to be suitable for printing;
S22, turning on a power switch, and adjusting a pressure regulator of the electric heating plate until the temperature of the baking sheet plate is 90-100 ℃;
s23, neatly and lightly placing the mica sheets into a printing hopper, and carrying out small placement each time to avoid damaging the mica sheets;
S24, sucking the mica sheet on a workbench, enabling a vacuum rubber brush to be stuck with a proper amount of silver paste, pressing down a frame stuck with a printing screen, and uniformly scraping the frame on a screen by flat lifting;
s25, sucking the printed films on a film drying plate on an electric heating film, drying the films, pouring the films into a film storage disc, printing the reverse side after all the films in a hopper are printed, paying attention to the fact that two silver layers are overlapped when the reverse side is printed, and printing the two silver layers of each batch of films by using a template;
step eight: sintering and infiltrating:
S31, checking whether the furnace temperature reaches the prescribed 280-300 ℃;
S32, scattering the rectangular sheets subjected to double-sided printing on a metal net disc, and putting the rectangular sheets into a infiltration furnace for infiltration, wherein the first time of low temperature is 300 ℃, and the sintering is carried out for 10 minutes;
S33, after the low-temperature sintering, checking and separating according to different types and thicknesses, performing sintering permeation at the high temperature of 570+/-10 ℃ for 2-3 minutes on qualified mica sheets after checking and separating, and then dragging the mica sheets to a furnace mouth for 2 minutes and taking out;
Step nine: slicing: cutting off the non-discolored part in the step, namely subtracting an inner frame size (12+/-0.3) X (12+/-0.3) part of the screen frame from a size specification 14X14, so that the final finished product is a discolored mica sheet;
The silver paste preparation method in the fifth step comprises the following steps:
s41, preparing silver paste for printing, wherein the raw materials are weighed according to the following components:
1400-1600 parts of silver mud,
The adhesive agent 500-700 is used as a binder,
100-300 Parts of terpineol,
30.5 To 32.5 percent of bismuth oxide,
20-28 Parts of lead borate,
80-120 Parts of ethylene glycol diethyl ether;
S42, putting silver paste raw materials to be prepared into a porcelain bottle;
s43, tightly covering and sealing, and then placing the ceramic balls on a ball mill for operation, wherein the ceramic balls are prevented from being broken during operation;
s44, controlling the ball milling time to be 100+/-10 hours, and controlling the running speed of the ball mill to be 75+/-5 rpm;
S45, filtering the sample test piece with a 170-180 mesh sieve after the sample test piece is normal, and storing the sample test piece in a clean and light-proof environment for later use;
the adhesive comprises the following components in percentage by weight: 250-270g of terpineol, 35-50g of ethyl cellulose and 460-470g of ethylene glycol diethyl ether;
The preparation method of the silver mud specifically comprises the following steps:
S51, weighing 950-1000g of silver carbonate powder, pouring the silver carbonate powder into a stainless steel pot, pouring 1700-1800me of n-butanol, heating and stirring;
S52, when the temperature is raised to 80-90 ℃, pouring 4-5g of rosin powder and 4.5-6.5g of collodion, and continuously stirring;
S53, dropwise adding 78-79g of n-butanol and 78-79g of triethanolamine by using a separating funnel when the temperature reaches 90-95 ℃, stopping heating, keeping the temperature at 93+/-1 ℃ for 2-3 hours, and keeping the temperature for 45-50 minutes, wherein the temperature is still 93+/-1 ℃;
s54, taking out silver mud, cooling for 10-12 hours, washing with absolute ethyl alcohol for 5-6 times, removing impurities, then placing in a ventilation opening, naturally drying, and grinding and storing the dried silver mud;
s55, placing the crushed silver mud in a place which is dry, light-proof and clean to prevent dust;
the preparation method of the silver carbonate powder specifically comprises the following steps:
s61, weighing 5-7g of rosin, grinding into powder, adding 50-58g of 99.5% ethanol for several days, and dissolving into yellowish brown liquid, namely 9% rosin water;
s62, adding 150-170me of distilled water into 35-45g of sodium carbonate, heating to fully dissolve the sodium carbonate into colorless transparent sodium carbonate solution, and cooling for later use;
S63, adding 250-300me of distilled water into 100-140g of silver nitrate, stirring for 15-20 minutes, pouring 10-14me of rosin water, and continuously stirring for a plurality of minutes, wherein the rotating speed of a stirrer is 160-180 revolutions per minute;
s64, gradually dripping the sodium carbonate solution into the silver nitrate solution by using a separating funnel, stopping adding the sodium carbonate solution when the reactant is alkaline after dripping the 1% phenolphthalein solution into pink after finishing dripping for 2-3 hours, and continuously stirring for a plurality of minutes;
S65, spreading filter paper in a porcelain funnel, pouring the prepared silver carbonate solution for filtering, flushing with distilled water and suction-filtering until the washing liquid is not alkaline, and dripping 1% phenolphthalein solution into the discharged washing water until the washing liquid is not red;
S66, placing the washed silver carbonate powder in an oven at 55-60 ℃ for drying for 5-7 days until no water exists, so that the silver carbonate is light yellow powder.
2. The method for changing color of mica flakes by silver spraying heat treatment according to claim 1, wherein the method comprises the following steps: the size specification grading of the mica sheet in the first step is as follows: 7X14, 12X12, 14X14, 16X16, 10X20, 19X25, 25X25, 20X30, 13X29, 17X34, 20X34, 30X40, 40X50; in the second step, the thickness grading of the mica sheet is as follows: the first gear is 14-16 μm, the second gear is 17-19 μm, the third gear is 20-22 μm, the fourth gear is 22-24 μm, the fifth gear is 26-30 μm, the sixth gear is 31-35 μm, the seventh gear is 36-40 μm, and the eighth gear is 41-45 μm.
3. The method for changing color of mica flakes by silver spraying heat treatment according to claim 1, wherein the method comprises the following steps: the preparation method of the adhesive comprises the steps of weighing 250-270g of terpineol, 40-45g of ethyl cellulose and 450-470g of ethylene glycol diethyl ether, mixing and stirring until the ethyl cellulose is completely dissolved.
4. The method for changing color of mica flakes by silver spraying heat treatment according to claim 1, wherein the method comprises the following steps: removing green, black, spots, impurities, bubbles, unevenness and mica sheets with low utilization rate which account for more than 5% of the total area of the mica sheets when the mica sheets are selected, and repairing serious burrs, cracks and unevenness parts at the edges of the mica sheets; when the mica sheet is peeled, uneven thickness and cracks of the mica edge are removed, and if bubbles are found, a puncture needle is used for puncturing a small hole.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR750290A (en) * | 1932-02-24 | 1933-08-08 | Rca Corp | Mosaic electrode refinements |
| CN103165217A (en) * | 2011-12-14 | 2013-06-19 | 上海宝银电子材料有限公司 | Electric conduction silver paste for mica plate capacitor and preparation method thereof |
| CN112126253A (en) * | 2020-09-14 | 2020-12-25 | 广东华彩顺成装饰材料有限公司 | Preparation method of blue mica pearlescent pigment and printing method of printed matter |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR750290A (en) * | 1932-02-24 | 1933-08-08 | Rca Corp | Mosaic electrode refinements |
| CN103165217A (en) * | 2011-12-14 | 2013-06-19 | 上海宝银电子材料有限公司 | Electric conduction silver paste for mica plate capacitor and preparation method thereof |
| CN112126253A (en) * | 2020-09-14 | 2020-12-25 | 广东华彩顺成装饰材料有限公司 | Preparation method of blue mica pearlescent pigment and printing method of printed matter |
Non-Patent Citations (1)
| Title |
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| 第四机械工业部标准化研究所."阻、容元件材料手册".1979,第244-251页. * |
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