CN1597137A - Poly-p-xylene surface coating equipment of ancient books and literatures and its coating technology - Google Patents
Poly-p-xylene surface coating equipment of ancient books and literatures and its coating technology Download PDFInfo
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- CN1597137A CN1597137A CN 200410041694 CN200410041694A CN1597137A CN 1597137 A CN1597137 A CN 1597137A CN 200410041694 CN200410041694 CN 200410041694 CN 200410041694 A CN200410041694 A CN 200410041694A CN 1597137 A CN1597137 A CN 1597137A
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Abstract
A vapour phase deposition technology for coating polyparaxylene onto the surface of ancient book's pages includes such steps as loading the polyparaxylene in evaporating tray, clamping the ancient book on its supporting frame, vacuumizing, heating the cracking to 600-700 deg.C, opening cold trap, heating evaporating chamber regulating throttle, turning on motor to rotate the supporting frame of book, and depositing the vapour of polyaraxylene on the surface of page. Its apparatus is also disclosed.
Description
Technical field
The Parylene surface applied equipment of ancient book of the present invention and document and coated technique thereof relate to is the vapour deposition coating technology and the coating device thereof of surperficial Parylene (Parylene) reinforcement protections such as ancient book (rare book ancient books) and archives, document.
Background technology
According to National Library the rotten present situation of China's collection book document paper aging is researched and analysed as can be known, documents such as China collection figure books and periodicals have been in comparatively serious ageing state at present, particularly the document paper aging before the forties in last century is particularly serious, can not circulating of having borrowed, take emergency measures will cause irretrievable loss as untimely, in February, 2004, Nanjing Library ancient books portion sent the urgent appeal of rescuing ancient book and the Republic of China's document in Jiangsu Province's Chinese People's Political Consultative Conference, point out that an ancient book faces the badly damaged circumstances frequently surplus the south figure existing 2,350,000, according to incompletely statistics, the ancient book that provincial library, the whole nation is in same condition surpasses 20000, they all the utmost point need wait for repairing and reinforcement.At present the ancient book of resident usefulness rescues guard method and mainly contains miniature, depickling reinforcing and silk net reinforcing etc., and the major defect of these methods is:
1, miniature: duplicating of document is the reproducibility safeguard measure of document, also can't carry out but the document that can't stir too serious embrittlement is miniature, and this miniature method can not keep the original appearance feature of ancient book.
2, depickling is reinforced: depickling is the important measures that delay book document aged deterioration speed, but there are problems such as cost height, complicated operation and environmental pollution in present acid stripping method.
3, silk net reinforcing: its major defect is that repair rate is too low, and workload is too big, and the life-span is not long.
In sum, known ancient book and document preservation reinforcement means are because technology and material itself are difficult to satisfy current urgent day by day ancient book and the Republic of China's document rescue situation requirement.
Parylene (Parylene) is to have unique a kind of high-tech performance materials by the preparation of vapour deposition (CVD) technology in the macromolecular material of practical value at present.Mainly comprise three kinds of structures (N type, C type, D type) in actual the use.The most basic structure is called ParyleneN, i.e. Parylene, and its structure is as follows:
Parylene C is a chloro polyxylene, is made of identical monomer, just one of them aromatic hydrocarbon hydrogen atom is replaced with a chlorine atom, and structural formula is as follows:
ParyleneN is a kind of highly crystalline structural material of complete linearity; it is a kind of good dielectric material; high insulation resistance is arranged and not with the dielectric constant of frequency change; it is the highest a kind of of penetration capacity among all Parylene; Parylene C combines good electrical properties, physical property; and have extremely low permeability for moisture content and other corrosive gas, what real free of pinholes can be provided covers the shape protection.Therefore, Parylene C is the preferred material of coating, as is applied in and is coated on paper surface, just can make books and document not be subjected to the invasion and attack of humidity and corrosive atmosphere, prolongs the life-span of books and document greatly.
Summary of the invention
The objective of the invention is to provide the Parylene surface applied equipment and the coated technique thereof of a kind of ancient book and document at above-mentioned weak point; it is the new method that rare book ancient books and the Republic of China's document preservation are repaired; enforcement through Parylene (Parylene) gas-phase deposition technology; making Parylene compound with the paper of books and document securely is one; it has not only kept ancient book (rare book ancient books) and archives; former states such as document; and greatly improved the efficient of repairing; can realize the batch reparation of books or document; and guarantee to prolong more than life-span to 500 year of book document; not only repairing effect is good; cost is low; economical and practical, be fit to China's national situation and catch up with and surpass the international high standards.
The Parylene surface applied equipment of ancient book and document and coated technique thereof take following scheme to realize: the Parylene surface applied equipment of ancient book and document comprises vaporization chamber, cracking room, polymerization settling chamber, cold-trap, choke valve, vacuum mechanical pump, refrigeration machine.Vaporization chamber has stainless steel evaporation cavity, at stainless steel evaporation cavity external body device electric heating tube is arranged, and at the evaporation indoor set evaporation boat is arranged, and vaporization chamber is connected with cracking room by pipeline.Cracking room has stainless steel cracking cavity, in stainless steel cracking cavity outside electric heating tube is housed, and cracking room is connected with the polymerization settling chamber by pipeline.
Polymerization settling chamber structure has vacuum bell jar, and vacuum bell jar is provided with observation window.Be provided with gas diverter in the vacuum bell jar, the gas diverter inlet links to each other with the outlet of cracking room tube connector, and gas diverter has the gas diverter cylindrical shell, the upper and lower sealing of cylindrical shell, be distributed with the gas tap hole of different flow resistances in cylindrical shell one side, to reach the cavity purpose that is evenly distributed.Part device has the books stent in vacuum bell jar, and the books stent links to each other with driving motor through the vacuum seal transmission mechanism, and the vacuum seal transmission mechanism has power transmission shaft, and device has vaccum seal ring on the power transmission shaft.Device has several books anchor clamps on the books stent, guarantees the books fanning, and gas diverter is provided with slide block.The books of clamping rotate on the books stent when application job, by slide block the books page are stirred and are opened, and make Parylene even in books page surface applied.Device has supervising device on the books stent, and with monitoring overlay quality, overlay thickness, supervising device adopts transparent glass tube, and by fixed bar, device is on the books stent.
Cold-trap import department is connected with the polymerization settling chamber by pipeline, and cold-trap exit device has choke valve, and vacuum mechanical pump links to each other with choke valve by pipeline.Cold-trap is connected with refrigeration machine, provides the circulation low-temperature receiver to cold-trap, makes the cold-trap cryogenic temperature reach-100 ℃.
The Parylene surface applied technology of ancient book and document may further comprise the steps:
1, the paraxylene raw material is contained in the evaporation boat in the vaporization chamber;
2, books that will apply or document clamping are on the books stent of polymerization settling chamber, and vacuum bell jar closes;
3, open choke valve, open vacuum mechanical pump, system is vacuumized, when the system vacuum degree reaches below the 10pa;
4, cracking room is warmed up to 600 ℃-700 ℃, open cold-trap, condenser temperature is reached below-80 ℃, and the heating evaporation chamber makes vaporization chamber be warming up to 120 ℃-125 ℃ steadily again, when surpassing 90 ℃, the vaporization chamber temperature regulates the choke valve pumping speed, make mud chamber's vacuum remain on 20-40pa, start driving motor simultaneously, make the rotation of books stent, speed is controlled at per minute 2-8 changes, and slide block begins to stir page;
5, the paraxylene gas that is produced by vaporization chamber enters cracking room, becomes activated monomer, enters the polymerization settling chamber by gas diverter, aggregates into Parylene at paper surface.Make in the polymerization settling chamber distribution of gas even by gas shunting, and allow Parylene be coated in the books or the document surface of rotation;
6, be used for supervising device by the observation window on the vacuum bell jar, mainly observe the glass tube transparency of supervising device, to guarantee the coated technique quality;
7, require between 120 ℃-125 ℃ of the control vaporization chambers according to every batch of books or document applied thickness, the coating time, long more applied thickness was thick more, and applied thickness is 4-10 μ m, and control speed is 1 μ m/ hour;
8, vaporization chamber cooling after coating finishes, when temperature drops to below 100 ℃, cracking room is lowered the temperature again, reduce to when the cracking room temperature and to close refrigeration machine below 600 ℃, close driving motor, and open choke valve, be lower than 350 ℃ until the cracking room temperature, can close choke valve, stop the vacuum machine pump work;
9, be lower than 200 ℃ when the cracking room temperature, promptly can open polymerization settling chamber vent valve, open vacuum bell jar, and measure the transparent glass tube coating film thickness of supervising device, the thickness that records is the thickness of coated books or document.
The Parylene surface applied equipment of ancient book and document and the characteristics of coated technique thereof are: in technique scheme, owing to adopt gas diverter to make the indoor gas of the gas precipitation state that is evenly distributed, to guarantee the uniformity and the uniformity of the thickness of books deposition coating in batches.Regulate choke valve both guaranteed the big capacity surface adsorbed gas of books in batches before coating by abundant desorption, when also having guaranteed the Parylene coating polymerizable gas in the abundant polymerization on books surface, guarantee coating in conjunction with effect.Supervising device is a kind of simple and easy monitoring arrangement that monitors the gas aggradation coating quality, and it can observe the rete transparency of coating process at any time, can carry out the measurement of applied thickness again after coating finishes.Books stent and slide block are the isolated plants of realizing that books apply in batches, increase the quantity of every batch of coating greatly.
Description of drawings
The invention will be further described below with reference to accompanying drawing.
Fig. 1 is the Parylene surface applied equipment schematic diagram of ancient book and document.
The specific embodiment
With reference to accompanying drawing 1, the Parylene surface applied equipment of ancient book and document comprises vaporization chamber 1, cracking room 5, polymerization settling chamber 9, cold-trap 20, choke valve 21, vacuum mechanical pump 22, refrigeration machine 19.Vaporization chamber 1 has stainless steel evaporation cavity 4, at stainless steel evaporation cavity 4 external device (ED)s electric heating tube 2 is arranged, and device has evaporation boat 3 in vaporization chamber 1, and vaporization chamber 1 is connected with cracking room 5 by pipeline 23.Cracking room 5 has stainless steel cracking cavity 7, in stainless steel cracking cavity 7 outsides electric heating tube 6 is housed, and cracking room is connected with polymerization settling chamber 9 by pipeline 24.
Cold-trap 20 import departments are connected with polymerization settling chamber 9 by pipeline 14, and cold-trap 20 exit devices have choke valve 21, and vacuum mechanical pump 22 links to each other with choke valve 21 by pipeline.Cold-trap 20 is connected with refrigeration machine 19, the circulation low-temperature receiver is provided for cold-trap 20, makes the cold-trap cryogenic temperature reach-100 ℃.
Embodiment 1:
The Parylene surface applied technology of ancient book and document may further comprise the steps:
1, the paraxylene raw material is contained in the evaporation boat in the vaporization chamber;
2, books that will apply or document clamping are on the books stent of polymerization settling chamber, and vacuum bell jar closes;
3, open choke valve, open vacuum mechanical pump, system is vacuumized, when the system vacuum degree reaches below the 10pa;
4, cracking room is warmed up to 600 ℃, open cold-trap, condenser temperature is reached below-80 ℃, and the heating evaporation chamber makes vaporization chamber be warming up to 120 ℃ steadily again, when surpassing 90 ℃, the vaporization chamber temperature regulates the choke valve pumping speed, make mud chamber's vacuum remain on 20pa, start driving motor simultaneously, make the rotation of books stent, speed is controlled at per minute 8 changes, and slide block begins to rotate page;
5, the paraxylene gas that is produced by vaporization chamber enters cracking room, become activated monomer, enter the polymerization settling chamber by gas diverter, aggregate into Parylene at paper surface, make in the polymerization settling chamber distribution of gas even by gas shunting, and allow Parylene be coated in the books or the document surface of rotation;
6, be used for supervising device by the observation window on the vacuum bell jar, mainly observe the glass pipe transparency of supervising device, to guarantee the coated technique quality;
7, require 120 ℃ of control vaporization chambers according to every batch of books or document applied thickness, the coating time, long more applied thickness was thick more, and applied thickness is 4 μ m, and control speed is about 1 μ m/ hour;
8, vaporization chamber cooling after coating finishes, when temperature drops to below 100 ℃, cracking room is lowered the temperature again, reduce to when the cracking room temperature and to close refrigeration machine below 600 ℃, close driving motor, and open choke valve, be lower than 350 ℃ until the cracking room temperature, can close choke valve, stop the vacuum machine pump work;
9, be lower than 200 ℃ when the cracking room temperature, promptly can open polymerization settling chamber vent valve, open vacuum bell jar, and measure the transparent glass tube coating film thickness of supervising device, the thickness that records is the thickness of coated books or document.
Embodiment 2:
The Parylene surface applied technology of ancient book and document may further comprise the steps:
1, the paraxylene raw material is contained in the evaporation boat in the vaporization chamber;
2, books that will apply or document clamping are on the books stent of polymerization settling chamber, and vacuum bell jar closes;
3, open choke valve, open vacuum mechanical pump, system is vacuumized, when the system vacuum degree reaches below the 10pa;
4, cracking room is warmed up to 700 ℃, open cold-trap, condenser temperature is reached below-80 ℃, and the heating evaporation chamber makes vaporization chamber be warming up to 125 ℃ steadily again, when surpassing 90 ℃, the vaporization chamber temperature regulates the choke valve pumping speed, make mud chamber's vacuum remain on 40pa, start driving motor simultaneously, make the rotation of books stent, speed is controlled at per minute 2 changes, and slide block begins to rotate page;
5, the paraxylene gas that is produced by vaporization chamber enters cracking room, become activated monomer, enter the polymerization settling chamber by gas diverter, aggregate into Parylene at paper surface, make in the polymerization settling chamber distribution of gas even by gas shunting, and allow Parylene be coated in the books or the document surface of rotation;
6, be used for supervising device by the observation window on the vacuum bell jar, mainly observe the glass pipe transparency of supervising device, to guarantee the coated technique quality;
7, require between 125 ℃ of the control vaporization chambers according to every batch of books or document applied thickness, the coating time, long more applied thickness was thick more, and applied thickness is 10 μ m, and control speed is about 1 μ m/ hour;
8, vaporization chamber cooling after coating finishes, when temperature drops to below 100 ℃, cracking room is lowered the temperature again, reduce to when the cracking room temperature and to close refrigeration machine below 600 ℃, close driving motor, and open choke valve, be lower than 350 ℃ until the cracking room temperature, can close choke valve, stop the vacuum machine pump work;
9, be lower than 200 ℃ when the cracking room temperature, promptly can open polymerization settling chamber vent valve, open vacuum bell jar, and measure the transparent glass tube coating film thickness of supervising device, the thickness that records is the thickness of coated books or document.
Two kinds of the Republic of China's Ta Kung Pao in period paper the Parylene surface applied equipment that uses ancient book of the present invention and document and coated technique thereof being handled by Jiangsu Province's quality technical supervision paper printing product quality inspection station and the Republic of China's Ta Kung Pao in period paper of uncoated Parylene compare detection, its tensile strength, folding strength, tearability are compared, the result shows: the newspaper in the Republic of China period is after Parylene (parylene) coating is reinforced, and its folding strength is better than the folding strength of present domestic paper greatly.In addition, its tensile strength and tearability also substantially exceed the paper of uncoated.Temperature degradation standard: 105 ℃ of oven temperatures, placed 12 days, do tensile strength, folding strength, tearability detection after the taking-up, qualified is 100 years; 105 ℃ of oven temperatures were placed 24 days, did tensile strength, folding strength, tearability detection after the taking-up, and qualified is 200 years; Oven temperature was placed 60 days for 105 ℃, did tensile strength, folding strength, tearability detection after the taking-up, and qualified is 500 years.Temperature aging life-span testing result shows, applies the paper life-span of reinforcing above 500 years through Parylene (parylene).
See Jiangsu Province's quality technical supervision paper printing product quality inspection station survey report:
Jiangsu Province's quality technical supervision paper printing product quality inspection station survey report
The sample title | Technical indicator | Unit | Assay | The method of inspection |
1937.3.8 and 3.9 Ta Kung Pao newspapers (unguyed) | Tensile strength | N | Vertical: 14.0 horizontal strokes: 8.8 | GB/T453-2002 |
Folding strength | Inferior | Vertical: 1.0 horizontal strokes: 0.3 | GB/T457-2002 | |
Tearability | MN | Vertical: 117 horizontal strokes: 136 | GB/T455-2002 | |
1937.3.7 and 3.12 Ta Kung Pao newspapers (are used ParyleneReinforce) | Tensile strength | N | Vertical: 35.5 horizontal strokes: 27.3 | GB/T453-2002 |
Folding strength | Inferior | Vertical: 1.86 horizontal strokes: 1.71 | GB/T457-2002 | |
Tearability | MN | Vertical: 151 horizontal strokes: 194 | GB/T455-2002 | |
Remarks | 1, entrust requirement only to provide measured data to committee's inspection project; 2, folding strength result: unguyed sample only can be measured the result 1 time on a small quantity, most of result that can not survey; Reinforce sample: vertically be up to 4 times, minimum 1 time, laterally be up to 3 times, minimum be 1 time; 3, sample is the Republic of China's Ta Kung Pao in period newspaper (March nineteen thirty-seven), and reinforcing all is 10 of this newspapers, and unguyed is 2 of this newspapers. |
Claims (6)
1, the Parylene surface applied equipment of a kind of ancient book and document is characterized in that structure comprises vaporization chamber, cracking room, polymerization settling chamber, cold-trap, choke valve, vacuum mechanical pump, refrigeration machine; Vaporization chamber has stainless steel evaporation cavity, at stainless steel evaporation cavity external body device electric heating tube is arranged, at the evaporation indoor set evaporation boat is arranged, vaporization chamber is connected with cracking room by pipeline, cracking room has stainless steel cracking cavity, in stainless steel cracking cavity outside electric heating tube is housed, cracking room is connected with the polymerization settling chamber by pipeline, polymerization settling chamber structure has vacuum bell jar, be provided with gas diverter in the vacuum bell jar, the gas diverter inlet links to each other with cracking room tube connector inlet, part device has the books stent in vacuum bell jar, and the books stent links to each other with driving motor through the vacuum seal transmission mechanism, and device has several books anchor clamps on the books stent, gas diverter is provided with slide block, and device has supervising device on the books stent.
2, the Parylene surface applied equipment of ancient book according to claim 1 and document is characterized in that gas diverter has the gas diverter cylindrical shell, and the upper and lower sealing of cylindrical shell is distributed with the gas tap hole of different flow resistances in cylindrical shell one side.
3, the Parylene surface applied equipment of ancient book according to claim 1 and document is characterized in that the vacuum seal transmission mechanism has power transmission shaft, and device has vaccum seal ring on the power transmission shaft.
4, the Parylene surface applied equipment of ancient book according to claim 1 and document is characterized in that supervising device adopts transparent glass tube, and by fixed bar, device is on the books stent.
5, the Parylene surface applied equipment of ancient book according to claim 1 and document is characterized in that vacuum bell jar is provided with observation window.
6, the Parylene surface applied technology of described ancient book of claim 1 and document is characterized in that coated technique may further comprise the steps:
(1) the paraxylene raw material is contained in the evaporation boat in the vaporization chamber;
(2) books that will apply or document clamping are on the books stent of polymerization settling chamber, and vacuum bell jar closes;
(3) open choke valve, open vacuum mechanical pump, system is vacuumized, when the system vacuum degree reaches below the 10pa;
(4) cracking room is warmed up to 600 ℃-700 ℃, open cold-trap, condenser temperature is reached below-80 ℃, and the heating evaporation chamber makes vaporization chamber be warming up to 120 ℃-125 ℃ steadily again, when surpassing 90 ℃, the vaporization chamber temperature regulates the choke valve pumping speed, make mud chamber's vacuum remain on 20-40pa, start driving motor simultaneously, make the rotation of books stent, speed is controlled at per minute 2-8 changes, and slide block begins to stir page;
(5) the paraxylene gas that is produced by vaporization chamber enters cracking room, become activated monomer, enter the polymerization settling chamber by gas diverter, aggregate into Parylene at paper surface, make in the polymerization settling chamber distribution of gas even by gas shunting, and allow Parylene be coated in the books or the document surface of rotation;
(6) be used for supervising device by the observation window on the vacuum bell jar, mainly observe the glass tube transparency of supervising device, to guarantee the coated technique quality;
(7) require between 120 ℃-125 ℃ of the control vaporization chambers according to every batch of books or document applied thickness, the coating time, long more applied thickness was thick more, and applied thickness is 4-10 μ m, and control speed is about 1 μ m/ hour;
(8) vaporization chamber cooling after coating finishes, when temperature drops to below 100 ℃, cracking room is lowered the temperature again, reduce to when the cracking room temperature and to close refrigeration machine below 600 ℃, close driving motor, and open choke valve, be lower than 350 ℃ until the cracking room temperature, can close choke valve, stop the vacuum machine pump work;
(9) be lower than 200 ℃ when the cracking room temperature, promptly can open polymerization settling chamber vent valve, open vacuum bell jar, and measure the transparent glass tube coating film thickness of supervising device, the thickness that records is the thickness of coated books or document.
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CN102115876A (en) * | 2009-12-31 | 2011-07-06 | 财团法人工业技术研究院 | Chemical vapor deposition device and method for forming poly-p-xylylene film |
CN104043566A (en) * | 2013-03-15 | 2014-09-17 | 三星显示有限公司 | Coating apparatus |
US8889224B2 (en) | 2009-12-18 | 2014-11-18 | Industrial Technology Research Institute | Method of forming parylene film |
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CN105039935A (en) * | 2015-08-24 | 2015-11-11 | 深圳市星火辉煌***工程有限公司 | Macromolecule vacuum covering device |
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CN115710836A (en) * | 2022-10-24 | 2023-02-24 | 国网浙江省电力有限公司电力科学研究院 | Method for improving insulation aging resistance of vegetable oil paper |
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US8889224B2 (en) | 2009-12-18 | 2014-11-18 | Industrial Technology Research Institute | Method of forming parylene film |
CN102115876A (en) * | 2009-12-31 | 2011-07-06 | 财团法人工业技术研究院 | Chemical vapor deposition device and method for forming poly-p-xylylene film |
CN104043566A (en) * | 2013-03-15 | 2014-09-17 | 三星显示有限公司 | Coating apparatus |
CN104043566B (en) * | 2013-03-15 | 2018-06-08 | 三星显示有限公司 | Coating unit |
CN104233228A (en) * | 2014-07-18 | 2014-12-24 | 许昌学院 | Full-automatic non-contact vacuum coating method and equipment |
CN105039935A (en) * | 2015-08-24 | 2015-11-11 | 深圳市星火辉煌***工程有限公司 | Macromolecule vacuum covering device |
CN110462094A (en) * | 2017-03-24 | 2019-11-15 | 艾克斯特朗欧洲公司 | For reducing the device and method of the partial pressure of water in OVPD Coating installation |
WO2023127644A1 (en) * | 2021-12-27 | 2023-07-06 | 東レ株式会社 | Method for manufacturing aromatic hydrocarbon, method for manufacturing polymer, and apparatus for manufacturing aromatic hydrocarbon |
CN115710836A (en) * | 2022-10-24 | 2023-02-24 | 国网浙江省电力有限公司电力科学研究院 | Method for improving insulation aging resistance of vegetable oil paper |
CN115710836B (en) * | 2022-10-24 | 2023-12-12 | 国网浙江省电力有限公司电力科学研究院 | Method for improving insulation ageing resistance of vegetable oil paper |
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