CN101109692B - Metallic film test piece and its preparing method for estimating and screening museum exhibition stuff - Google Patents
Metallic film test piece and its preparing method for estimating and screening museum exhibition stuff Download PDFInfo
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- CN101109692B CN101109692B CN2007100451932A CN200710045193A CN101109692B CN 101109692 B CN101109692 B CN 101109692B CN 2007100451932 A CN2007100451932 A CN 2007100451932A CN 200710045193 A CN200710045193 A CN 200710045193A CN 101109692 B CN101109692 B CN 101109692B
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Abstract
The present invention pertains to the technical field of material testing, in particular to a metallic film specimen and its preparing method for evaluating and screening the stored materials in a museum. The invention uses modern and mature film-coating technology to coat silver and copper particle film in thickness of 100-300nm on surfaces of different substrates, so as to get the desired metallic film specimen. The invention can greatly reduce the use of metallic material, simplify operation and reduce cost; can avoid the shortcoming of poor repeatability of experimental data due to bulk metallic specimen, is good for digital analysis on the difference in specimen before and after corrosion, and overcomes any artificial error brought about by Oddy Test due to observation by naked eyes, and cangreatly reduce the test period, is good for popularization and application in great scale.
Description
Technical field
The invention belongs to the testing of materials technical field, be specifically related to the collection exhibition materials assessment screening metallic film test piece and preparation method thereof of a kind of museum.
Background technology
Along with the development of modernization industry, it is more and more to be elected to be kinds such as storage, display and ornamental material such as timber, plastics, textile, coating, bonding agent, macromolecular material, compound substance for the museum.These storages, display and decoration can slowly discharge or degrade with material and generate various volatile ingredients, as sulfocompound, formic acid, acetate, alkene, carbonyls etc.And in the showcase or storeroom of sealing, these compound concentrations can constantly discharge increase and will speed up corrosion to historical relic such as various metal historical relics from material.Although people have carried out big quantity research to volatile matter with destruction and source thereof that museum's display ornament materials produces.But many museums all an urgent demand test the material that historical relic's protection is not had potential hazard to identify to the exhibition of hiding fast with material, so that from the corrosion of source prevention historical relic microenvironment to historical relic in it.
From at present domestic and international prior art; in order to detect the material that historical relic is had potential hazard; assessment is used to make material such as museum objects storehouse, showcase, storage cabinet and the museum's subenvironment adaptability to historical relic's protection, many research institutions a kind of corrosion test method---Oddy Test method that still the Britain museum proposes before adopting 30 years.The OddyTest method is a kind of accelerated corrosion experimental technique, be that measured material and the block test piece of the metal that exposes active surface through polishing are sealed in the same glass testing tube simultaneously, be 100% in relative humidity, 60 ℃ of temperature, reaction time be to test under 28 days the condition, and the extent of corrosion by metal testing plate come to measured material be suitable for long-term use, short-term is used or be not suitable for making and be used for classifying.
Though this method can obtain result comparatively reliably, help to assess the display ornament materials influences historical relic in a long period situation.But this method in use also exposes some shortcomings, and is oversize as test period, needs 28 days usually.If a kind of material not by test, then needs another kind of material to replace repeated experiments, make that whole test phase is long, this is unfavorable for the purchase of storage, display and ornament materials, whether uses in time and make decision; Used metal testing plate is the reguline metal of exposing active surface with sheet metal process glass brush or sand papering.In the bruting process of sheet metal, can cause the loss of raw material metal, and influencing metal testing plate smoothness of the surface and planarization, the physical distortion that is caused also can cause the error (hole point that general surface deformation after treatment or surperficial appearance can not grind off or dark road vestige just can not be used again) when estimating; Bruting process also can be introduced the metal surface with impurity.For this reason, usually the slight concussion washing in optical voidness acetone of the metal testing plate that will polish in the tradition Oddy Test testing procedure, not only used the high acetone of high-purity valency, and surface impurity will have residual, thereby influence the assessment result of historical relic collection exhibition materials; Adopt nylon wire to connect metal testing plate and hang in the airtight glass testing tube, also be unfavorable for test piece fixing or the like in the glass testing tube.For this reason, people have carried out some improvement to Oddy Test method.But up to the present, improvement to this method all is to realize as temperature, humidity, container size and shape etc. by changing other influence factors under the situation that does not change the reguline metal test piece, and the running program after improving also is based upon on traditional Oddy Test method trace routine basis.
Nano particle shows many special natures that are different from conventional blocks of solid such as small-size effect, surface effect and macro quanta tunnel effect usually.The preparation of metal nano material is one of focus in the present material preparation, especially nano level copper and nano level silver.Owing to characteristic such as the attention that enjoys people such as bigger serface and high surface of himself.28 days test duration of tradition Oddy Test method is the influence that it can find all corrosive substances in the tested sample, comprises whether material that measured material volatilized in the test process and the catabolite that degraded produced have corrosivity.And this high surface of nano particle is equivalent to a kind of accelerated corrosion process undoubtedly, may have quite high reaction sensibility to corrosivity composition (comprising catabolite), this develops a kind of method of retrofit testing fast and accurately and has created condition shortening the test duration.
In recent years, the study on the synthesis of relevant Nano Silver, copper has obtained very fast development, not only can prepare various different sizes, difform nano particle, and can prepare nano wire and the surperficial film that contains silver, copper nano-particle.Preparation method commonly used is divided into chemical method and physics method.Chemical method has sol-gel process, electrochemical plating, oxidation-reduction method, vacuum vapour deposition, supercritical ultrasonics technology, electrochemical process and radiation method etc.The I of the silver-colored particle of chemical method preparation reaches several nanometers, and is simple to operate, control easily.The physics method mainly is evaporation, sputter plating and the ion plating etc. under some vacuum, specifically comprises many types, as vacuum ionic evaporation, magnetron sputtering, molecular beam epitaxy, laser splash deposition etc.Evaporation coating in the middle of this generally is that the heating target makes surface component be evaporated out with atomic group or ionic species, and is deposited in substrate surface formation film.For sputter class plated film, then be to utilize electronics or superlaser bombardment target, surface component is sputtered out with atomic group or ionic species, finally be deposited on substrate surface and film forming.Wherein, magnetron sputtering plating then is that electronics quickens to fly under effect of electric field in the process of substrate and bumps with ar atmo, and ionization goes out a large amount of argon ions and electronics, and electronics flies to substrate.Argon ion quickens the bombardment target under effect of electric field, sputter a large amount of target atom, is neutral target atom (or molecule) and is deposited on film forming on the substrate.Above-mentioned these different nano thin-film preparation methods take a firm foundation for preparation silver, copper nano thin-film on various stromal surface such as glass sheet, piezoid, potsherd, plastic sheet, electrode surface.Based on studies show that of Ag film (8.2nm-107.2nm) that on glass sheet, prepare different-thickness with sputtering method, increase along with film thickness, the mean grain size size of film increases gradually, interplanar distance reduces gradually, membrane structure gradually becomes continuous film by discontinuous film, and its physical property tends towards stability.Therefore silver-plated, the copper film THICKNESS CONTROL of the present invention institute is at 100-300nm.
Summary of the invention
The object of the present invention is to provide short, easy and simple to handle metal testing plate that is used for museum's collection exhibition materials assessment screening of a kind of test period and preparation method thereof.
The metal testing plate that is used for museum collection exhibition materials assessment screening provided by the invention by plating silver or copper nanometer rete and obtain through the nano-coating technology on the substrate, is a kind of metallic film test piece; Described substrate is not for having corrosivity and surface to be suitable for the substrate of plated film to silver or copper, as glass sheet, organic glass sheet, the poly-right plastic sheet of second etc., it is shaped as diameter 18-25mm, thickness is the circle of 0.8-1.2mm, perhaps be the rectangle of long 20-35mm, wide 10-15mm, thick 1.5-2.5mm, the thickness of silver or copper film layer is 100-300nm.
The preparation method of above-mentioned metallic film test piece is as follows:
(1) clean substrate, one or more modes of adopt that washing agent is washed, nitric acid hydrogen peroxide mixed liquid dipping, distilled water ultrasonicly being washed, ethanol is ultrasonic in washing make up each ultrasonic 5-20 minute, after washing at every turn, wash,, dry processing then with the used solution of flush away;
(2) plated film adopts nano-coating technology plated film, for example modern ripe vacuum vapor plating, and magnetron sputtering plating, vacuum ion membrane plating or optical coating technology etc., the target that plated film is used is a purity greater than 99.9% silver or copper metal; The thickness of plated film is 100-300nm, specifically controls by the amount of controlling silver or copper, and the silver of promptly per 100 substrate consumption or copper amount are controlled in the 0.4-0.8g scope.
In the methods of the invention, selected substrate material need have heat resistance, with anti-deformation and softening.
In the methods of the invention, made substrate should be avoided surface abrasion and scuffing, so that the plated film program of back.
In the methods of the invention, made metallic film test piece needs vacuum-packed the preservation owing to have higher surface activity.
The inventive method has the following advantages:
(1) utilize the silver of substrates of different material, the test piece of copper nano thin-film to replace traditional reguline metal test piece, increase the metallic surface activity, improved the Oddy Test method of traditional British Museum, can shorten the time that collection exhibition materials is estimated significantly, effectively shorten the test period, realize shortening to about 14 days by 28 days.
(2) test piece that replaces the polishing of original Traditional bulk metal surface to form by the metallic film test piece can reduce raw-material consumption significantly, reduces experimentation cost.
(3) utilize modern advanced coating technique and equipment, can strictly control the various conditions of producing the film test piece, can guarantee thickness, compactness, homogeneity and the particle size of silver, copper film in the nano thin-film metal testing plate, and the cleanliness of test piece and smoothness, the acetone washing lotion need be do not passed through, the interference of other impurity can be prevented.
(4) adopt circular substrate or microscler substrate to replace former rectangular reguline metal test piece, help the suspension of test piece in the glass test bottle and fix and test later image collection, detection and analysis.
(5) compare with the use of original reguline metal test piece, the bruting process that test piece has been exempted in the direct use of silver, copper metal film test piece, and can give full play to the excellent specific property of nano metal particles self, its higher surface activity has been quickened corrosion process, has shortened the test duration.The industrialization of its lower cost, short test duration, standardization, standardization and achievement that characteristics easily and effectively help test piece.
Description of drawings
Fig. 1 is that the number of glass physa sheet and silver plating film test piece is gathered picture, wherein silver plating film test piece surface present black be since nano thin-film to due to the height reflection and scattering of light, the test piece of copper facing film also is like this.
Fig. 2 is scanning electron microscope (SEM) figure of silver-colored film test piece coating surface.
Fig. 3 is scanning electron microscope (SEM) figure of plating film test piece surface coating layer cross section.
Embodiment
Below by embodiment method provided by the invention is given further instruction, but not thereby limiting the invention.
Substrate for use among the embodiment: silver, copper metal are not had the corrosive and surperficial substrate that is suitable for plated film, as glass sheet, organic glass sheet, vinyon sheet etc., diameter is that 20.0mm, thickness are the circular substrate of 1.0mm, or long 20.0-35.0mm, wide 10.0-15.0mm, the microscler substrate of thick 2.0mm.
The cleaning of substrate: the detergent solution with heat washes → washes → and ethanol is ultrasonic to be washed → washes → and mixed solution immersion → washing → distilled water is ultrasonic washes → 110 ℃ of dry for standby for nitric acid hydrogen peroxide (volume ratio 1: 3).
Filming equipment: adopt vacuum evaporation, magnetron sputtering, filming equipments such as ion plating are as the DMD-450 type optical multilayer coating machine of Beijing instrument plant production.
The plated film target: purity is 〉=99.9% silver, copper metal.
Embodiment 1
Substrate: glass wafer
The plated film target: purity is 〉=99.9% silver
Filming equipment: the DMD-450 type optical multilayer coating machine of producing with Beijing instrument plant is an example
Film thickness monitoring: 0.4g/100 sheet glass disk
Be coated with process: open the coating machine vacuum chamber, 100 sheet glass disks are adhered on the coating machine bracket by high temperature gummed tape, put into coating machine behind the cleaning surfaces, and put into 0.4g purity and use parts in evaporating for 〉=99.9% silver.Close vacuum chamber and be evacuated to 1 * 10
-5Torr begins evaporation then.About 30-60 of plated film time minute.Open vacuum chamber after the end, can take off made test piece and vacuum-packed.The film thickness that is plated is approximately 100-200nm.
Embodiment 2
Substrate: glass wafer
The plated film target: purity is 〉=99.9% silver
Filming equipment: the DMD-450 type optical multilayer coating machine of producing with Beijing instrument plant is an example
Film thickness monitoring: 0.6g/100 sheet glass disk
Be coated with process: open the coating machine vacuum chamber, 100 sheet glass disks are adhered on the coating machine bracket by high temperature gummed tape, put into coating machine behind the cleaning surfaces, and put into 0.6g purity and use parts in evaporating for 〉=99.9% silver.Close vacuum chamber and be evacuated to 1 * 10
-5Torr begins evaporation then.About 30-60 of plated film time minute.Open vacuum chamber after the end, can take off made test piece and vacuum-packed.The film thickness that is plated is approximately about 200nm.
Embodiment 3
Substrate: plastic sheet
The plated film target: purity is 〉=99.9% silver
Filming equipment: the DMD-450 type optical multilayer coating machine of producing with Beijing instrument plant is an example
Film thickness monitoring: 0.6g/100 sheet plastic sheet
Be coated with process: open the coating machine vacuum chamber, 100 plastic sheets are adhered on the coating machine bracket by high temperature gummed tape, put into coating machine behind the cleaning surfaces, and put into 0.6g purity and use parts in evaporating for 〉=99.9% silver.Close vacuum chamber and be evacuated to 1 * 10
-5Torr begins evaporation then.About 30-60 of plated film time minute.Open vacuum chamber after the end, can take off made test piece and vacuum-packed.The film thickness that is plated is approximately about 200nm.
Embodiment 4
The measured material (is example with 5mm medium density fibre board (MDF)-plate 18) of about 2g is put into the glass testing tube container of the 50mL of tool ground, be cut into the bulk of about 10 * 10 * 5mm.0.5mL small test tube in pack into and seal with absorbent cotton behind the distilled water, put into test container.Cut apart with a knife or scissors the test piece of vacuum-packed silver metal film with scissors.Hand fetches the test piece of silver metal film after wearing double gloves (wearing the clean thin mitten of one deck again after wearing the disposable PE plastic glove of one deck), is clipped in outer being with on the stainless steel anchor clamps of polyfluortetraethylene pipe, and hangs in the corresponding hook.Standard grinding port plug surface twines skim teflon unsintered tape, is used for the further sealing of test container.Prepare a control test (adopt traditional silver bullion shape test piece, other are same as above) and a blank test (do not add test material, only add metallic film test piece and water) simultaneously.Test container is put into 60 ℃ of baking ovens.React after 14 days, take out the metallic film test piece.Adopt the stereoscopic micro-digital imaging system of XTL-3400 type to take pictures to testing test piece, and with the test piece contrast of two control tests.Found that two contrast all variations of test pieces, but actual test test piece has become blue and has carried white patch secretly, the appearance that demonstration is corroded.
Embodiment 5
Substrate: glass wafer
The plated film target: purity is 〉=99.9% copper
Filming equipment: the DMD-450 type optical multilayer coating machine of producing with Beijing instrument plant is an example
Film thickness monitoring: 0.4g/100 sheet glass disk
Be coated with process: open the coating machine vacuum chamber, 100 sheet glass disks are adhered on the coating machine bracket by high temperature gummed tape, put into coating machine behind the cleaning surfaces, and put into 0.4g purity and use parts in evaporating for 〉=99.9% copper.Close vacuum chamber and be evacuated to 1 * 10
-5Torr begins evaporation then.About 30-60 of plated film time minute.Open vacuum chamber after the end, can take off made test piece and vacuum-packed.The film thickness that is plated is approximately 100-200nm.
Embodiment 6
Substrate: glass wafer
The plated film target: purity is 〉=99.9% copper
Filming equipment: the DMD-450 type optical multilayer coating machine of producing with Beijing instrument plant is an example
Film thickness monitoring: 0.6g/100 sheet glass disk
Be coated with process: open the coating machine vacuum chamber, 100 sheet glass disks are adhered on the coating machine bracket by high temperature gummed tape, put into coating machine behind the cleaning surfaces, and put into 0.6g purity and use parts in evaporating for 〉=99.9% copper.Close vacuum chamber and be evacuated to 1 * 10
-5Torr begins evaporation then.About 30-60 of plated film time minute.Open vacuum chamber after the end, can take off made test piece and vacuum-packed.The film thickness that is plated is approximately about 180-300nm.
Embodiment 7
Substrate: plastic sheet
The plated film target: purity is 〉=99.9% copper
Filming equipment: the DMD-450 type optical multilayer coating machine of producing with Beijing instrument plant is an example
Film thickness monitoring: 0.6g/100 sheet plastic sheet
Be coated with process: open the coating machine vacuum chamber, 100 plastic sheets are adhered on the coating machine bracket by high temperature gummed tape, put into coating machine behind the cleaning surfaces, and put into 0.6g purity and use parts in evaporating for 〉=99.9% copper.Close vacuum chamber and be evacuated to 1 * 10
-5Torr begins evaporation then.About 30-60 of plated film time minute.Open vacuum chamber after the end, can take off made test piece and vacuum-packed.The film thickness that is plated is approximately about 200-300nm.
Embodiment 8
The measured material of about 2g (knit to be numbered-5 textile be example) is put into the glass testing tube container of the 50mL of tool ground, be cut into the bulk of about 10 * 10 * 5mm.0.5mL small test tube in pack into and seal with absorbent cotton behind the distilled water, put into test container.Cut apart with a knife or scissors vacuum-packed copper metal film test piece with scissors.Hand fetches the copper metal film test piece after wearing double gloves (wearing the clean thin mitten of one deck again after wearing the disposable PE plastic glove of one deck), is clipped in outer being with on the stainless steel anchor clamps of polyfluortetraethylene pipe, and hangs in the corresponding hook.Standard grinding port plug surface twines skim teflon unsintered tape, is used for the further sealing of test container.Prepare a control test (adopt traditional copper billet shape test piece, other are same as above) and a blank test (do not add test material, only add metallic film test piece and water) simultaneously.Test container is put into 60 ℃ of baking ovens.React after 14 days, take out the metallic film test piece.Adopt the stereoscopic micro-digital imaging system of XTL-3400 type to take pictures to testing test piece, and with the test piece contrast of two control tests.Found that block test piece no change, and actual test test piece has become blue and carried dark brown red secretly, shown the appearance that is corroded.
Claims (2)
1. museum's collection exhibition materials assessment screening metallic film test piece, it is characterized in that by plating silver or copper nanometer rete through the nano-coating technology on the substrate and obtain, described substrate is glass sheet, organic glass sheet or vinyon sheet, it is shaped as diameter 18-25mm, thickness is the circle of 0.8-1.2mm, perhaps be the rectangle of long 20-35mm, wide 10-15mm, thick 1.5-2.5mm, the thickness of silver or copper film layer is 100-300nm.
2. the preparation method who uses the metallic film test piece is screened in a museum as claimed in claim 1 collection exhibition materials assessment, it is characterized in that concrete steps are as follows:
(1) clean substrate, one or more modes of adopt that washing agent is washed, nitric acid hydrogen peroxide mixed liquid dipping, distilled water ultrasonicly being washed, ethanol is ultrasonic in washing make up each ultrasonic 5-20 minute, after washing at every turn, wash,, dry processing then with the used solution of flush away;
(2) plated film adopts nano-coating technology plated film, and the target that plated film is used is a purity greater than 99.9% silver or copper metal; The thickness of plated film is 100-300nm, specifically controls by the amount of controlling silver or copper.
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| EP4339592A1 (en) * | 2022-09-14 | 2024-03-20 | Hochschule für Technik und Wirtschaft Berlin | Analysis method with coated support |
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| CN101477025B (en) * | 2008-12-11 | 2011-08-31 | 西安交通大学 | Fast evaluation method for collection exhibition materials based on image processing |
| CN101968477B (en) * | 2010-08-27 | 2014-12-03 | 华南理工大学 | Medical integrated magnesium alloy biodegradability gas-collection measurement device |
| CN101921991A (en) * | 2010-09-07 | 2010-12-22 | 上海交通大学 | Plasma immersion ion injection method for improving anti-oxidation property of copper film |
| CN108572920B (en) * | 2017-03-09 | 2022-04-12 | 上海宝存信息科技有限公司 | Data moving method for avoiding read disturbance and device using same |
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| GB2430202A (en) * | 2005-09-20 | 2007-03-21 | Mantis Deposition Ltd | Antibacterial surface coatings |
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| GB2430202A (en) * | 2005-09-20 | 2007-03-21 | Mantis Deposition Ltd | Antibacterial surface coatings |
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| EP4339592A1 (en) * | 2022-09-14 | 2024-03-20 | Hochschule für Technik und Wirtschaft Berlin | Analysis method with coated support |
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