CN103570280A - Preparation method and reinforcement method of crispy powder ceramic culture relic reinforcement material - Google Patents
Preparation method and reinforcement method of crispy powder ceramic culture relic reinforcement material Download PDFInfo
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- CN103570280A CN103570280A CN201310011475.6A CN201310011475A CN103570280A CN 103570280 A CN103570280 A CN 103570280A CN 201310011475 A CN201310011475 A CN 201310011475A CN 103570280 A CN103570280 A CN 103570280A
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Abstract
The invention relates to a preparation method and a reinforcement method of a crispy powder ceramic culture relic reinforcement material. The preparation method comprises the following steps: mixing ethyl orthosilicate and hydroxyl terminated polydimethylsiloxane, and stirring for 12 to 24 hours; continuously stirring an obtained mixture for more than 5 minutes under the effect of a dibutyltin dilaurate catalyst so as to obtain the crispy powder ceramic culture relic reinforcement material.
Description
Technical field
The invention belongs to historical relic's protection field, relate to a kind of preparation method and reinforcement means of crisp powder relics reinforcement material.
Background technology
Pottery is one of innovation and creation the earliest in human history, and the invention of pottery is an important significant progress on history of human civilization.Ancient Chinese relics has one of the most valuable historical and cultural heritage that the distinct ancients of the feature ，Shi Chinese nation of the Chinese nation carry over.Ancient times, the development differentiation of relics was closely related with the mankind's production, life, it is in the development differentiation of nearly ten thousand years, witness the development course of Chinese civilization, it is the important carrier of historical information, invention and the progress of mankind's technology have been reflected, condense the intelligence and wisdom of the Chinese nation, for foundation and the division of history into periods developmental sequence of implements typology in archeological researches provides most important geological material foundation, there is irreplaceable artistic value, historical value and scientific value.
The protection situation of China's relics is very severe at present, State Cultural Relics Bureau has organized and implemented < < Ceramic Cultural Relics corrosion loss investigation > > project in 1999～2003 years, in the survey showed that ancient Chinese pottery, exist saltout, the disease such as surperficial crisp powder, glaze colours transformation, surperficial flaking, wearing and tearing; In " ceramic colored drawing historical relic's protection State Cultural Relics Bureau's emphasis scientific base " scientific research activity in 2006; investigation is learnt that Guanzhong area colored drawing relics carcass is preserved and good is not accounted for 41%; what preservation condition moderate was impaired has accounted for half, and wherein the crisp powder in relics surface has the greatest impact to the permanent preservation of historical relic.The unearthed relics of Longxian County of Shaanxi shop Qin Mu of take is example, and the crisp powder in pottery surface is serious, is bed separation, there is between layers obvious border, skin is thicker, hole is large and loose, and internal layer is relatively fine and close, and macroscopic white soluble salt crystalline particle appears in part surface; The soluble salts such as the sodium-chlor that research discovery ceramic sample contains, calcium chloride are to cause the crisp powder of cultural artifact surface, the major cause coming off.
For the main easy protectiveness treatment process of crisp powder relics, be to use protecting materials to carry out penetration reinforcement processing to historical relic at present; for fragile silicate cultural relic, conventionally adopt at present acrylate, organosilicon, organic fluorine, nano modified material and compound differing materials to carry out a series of rescue protection work both at home and abroad.For example CN100450974C discloses a kind of vacuum impregnation guard method of unearthed relics, and it adopts organic silicon composite to protect moisture unearthed relics as dipping protecting materials, CN101851113A discloses the guard method of a kind of native ruins, brick cultural relics and stone cultural artifact, adopts the nano inorganic silicon aqueous solution and inorganic silicon water-resisting agent, as protecting materials, historical relic is carried out to penetration reinforcement, bibliographical information has the tetraethyl silicate of employing and oligosiloxane protection Spain and gondola historic site, γ-(methacryloxypropyl) propyl trimethoxy silicane, polyhedral oligomeric silsesquioxane modification tetraethoxy material protection stone cultural artifact etc., but about the sodium-chlor containing, the reinforcement protecting material research report that the soluble salts such as calcium chloride cause crisp powder relics seldom, therefore obtain and there is certain depth of penetration, do not change and reinforce rear color sample, condition of surface, after reinforcing, sample strength and crisp powder ceramic sample matrices match simultaneously, and the research with the crisp powder relics reinforcement protecting material of the performances such as certain ventilation property and salt tolerant corrosion has importance and necessity.
Summary of the invention
Therefore, the object of the present invention is to provide a kind of reinforce crisp powder relics required there is certain depth of penetration, do not change reinforce after crisp powder relics color sample and condition of surface, reinforce crisp powder sample strength and ceramic sample matrices intensity matches simultaneously, and the preparation method with the reinforcement material of the performance requriementss such as certain ventilation property, thermostability and salt tolerant corrodibility, and the reinforcement material prepared of described preparation method is reinforced the reinforcement means of crisp powder relics.
At this, on the one hand, the invention provides a kind of preparation method of crisp powder relics reinforcement material, comprising: mix tetraethoxy and hydroxyl endblocked polydimethylsiloxane, stir 12～24 hours; And gained mixture continues to stir and within 5 minutes, makes above described crisp powder relics reinforcement material under the effect of dibutyltin dilaurate catalyst.
Described hydroxyl endblocked polydimethylsiloxane is a kind of linear reactive polysiloxanes, belongs to the functionalized silicon based polysiloxane that is directly connected with hydroxy functional group on straight chain, two sections of Siliciumatoms.In the present invention, the hydroxyl endblocked polydimethylsiloxane that preferred molecular weight is 400～1500, hydroxy radical content is 4～6%, viscosity is 32～45cst.It can be by further reaction is crosslinked with tetraethoxy.
Preferably, the consumption of described hydroxyl endblocked polydimethylsiloxane account for described tetraethoxy volume 5～10%.
Again, preferably, the consumption of described dibutyltin dilaurate catalyst account for tetraethoxy volume 1%.
Described stirring all adopts magnetic stirring apparatus; utilize the principle of magnetic field and whirlpool to drive the magnetic stir bar of putting into liquid to do circumference cyclic motion; thereby coordinate control temperature and rotating speed to reach the object of uniform stirring; shape of magnetic stir bar and consumption, viscosity and the carrying container of solution etc. is relevant, can not corrode by protected material.In the present invention, preferably, can coordinate and control 25 ℃ of temperature, rotating speed 400～600rpm.
On the other hand, the present invention also provides a kind of reinforcement means of crisp powder relics, comprising: in surface coverage, have and on the crisp powder relics of sorbing material, slowly add reinforcement material prepared by above-mentioned preparation method until described sorbing material is state of saturation; And be transferred in climatic chamber and preserve until described reinforcement material is completely curing.
In the present invention, the ultimate compression strength of described crisp powder relics is less than 10MPa, and opposing environment capacity is poor, does not have can support historical relic body intensity, need reinforcement after processing and could preserve for a long time.
Described sorbing material is natural or synthetic flexibility fabric, comprises cotton gauze, adsorption paper etc.
Preferably, can adopt needle tubing instillation or the banister brush spread coating of not damaging crisp powder surface slowly to add described reinforcement material.
Again, preferably, the temperature that can control described climatic chamber is 25 ℃, and relative humidity is 50%.
After reinforcing completes, be reinforced crisp powder relics outward appearance almost without changing, described reinforcement material is permeable to described crisp powder relics inside 3～6mm, and fastening strength improves.And be reinforced crisp powder relics and have certain water vapor transmission rate (WVTR), thermostability and Salt Corrosion are excellent.
Preparation method and the reinforcement means implementation and operation of crisp powder relics reinforcement material of the present invention are simple, use the method can make ultimate compression strength be less than 10MPa or local compressed strength is lower, the crisp powder relics that caused by soluble salt etc. obtains good reinforcement protection.
Accompanying drawing explanation
Fig. 1 is crisp powder relics reinforcement protecting material absorption spectrum curve;
Fig. 2 is crisp powder relics reinforcement protecting material microstructure.
Embodiment
Below in conjunction with following embodiment, further illustrate the present invention, should be understood that following embodiment is only for the present invention is described, and unrestricted the present invention.
The preparation method of crisp powder relics reinforcement material of the present invention comprises: mix tetraethoxy and hydroxyl endblocked polydimethylsiloxane, stir 12～24 hours; And gained mixture continues to stir and within 5 minutes, makes above described crisp powder relics reinforcement material under the effect of dibutyltin dilaurate catalyst.
The reinforcement means of crisp powder relics of the present invention comprises: in surface coverage, have and on the crisp powder relics of sorbing material, slowly add reinforcement material prepared by above-mentioned preparation method until described sorbing material is state of saturation; And be transferred in climatic chamber and preserve until described reinforcement material is completely curing.
In conjunction with above-mentioned preparation method and reinforcement means, more specifically, as example, the present invention can comprise the following steps.
(1) in tetraethoxy (TEOS), add the hydroxyl endblocked polydimethylsiloxane (PDMS-OH) that accounts for its volume fraction 5～10%, control 25 ℃ of heating magnetic agitation actuator temperatures, rotating speed 400～600rpm, add magnetic stir bar to stir after 12～24 hours, add and account for the stirring of the strong gelation dibutyl tin laurate of having of tetraethoxy volume fraction 1% (DBTL) catalyzer more than 5 minutes, synthetic crisp powder relics reinforcement material, its absorption spectrum curve is as shown in the grey solid line in Fig. 1, black solid line in Fig. 1 illustrates the absorption spectrum curve of contrast tetraethoxy (TEOS).Referring to Fig. 2, it illustrates the microstructure of synthetic crisp powder relics reinforcement material.
(2) in ultimate compression strength, be less than the crisp powder relics surface of 10MPa, cover the sorbing materials such as cotton gauze, adsorption paper, then adopt needle tubing instillation or banister brush spread coating slowly to add the prepared reinforcement material of step (1), until sorbing material is state of saturation, to after the crisp powder relics covered with plastic film parcel after processing, be positioned over 25 ℃ of temperature, in the climatic chamber of relative humidity 50%, preserve, until described reinforcement material is completely curing, for example, can preserve 1～2 week.
Hydroxyl endblocked polydimethylsiloxane in step (1) is a kind of linear reactive polysiloxanes, belong to the functionalized silicon based polysiloxane that is directly connected with hydroxy functional group on straight chain, two sections of Siliciumatoms, molecular weight 400～1500, hydroxy radical content 4～6%, viscosity 32～45cst, can be by further reaction is crosslinked with tetraethoxy.
Magnetic stirring apparatus in step (1); utilize the principle of magnetic field and whirlpool to drive the magnetic stir bar of putting into liquid to do circumference cyclic motion; thereby coordinate control temperature and rotating speed to reach the object of uniform stirring; shape of magnetic stir bar and consumption, viscosity and the carrying container of solution etc. is relevant, can not corrode by protected material.
Crisp powder relics in step (2), opposing environment capacity is poor, does not have can support historical relic body intensity, need reinforcement after processing and could preserve for a long time.
Method of the present invention has the following advantages and positively effect:
Be reinforced crisp powder relics outward appearance almost without changing, reinforcement material is permeable to crisp powder relics inside 3～6mm, and fastening strength improves, and has certain water vapor transmission rate (WVTR), and thermostability and Salt Corrosion are excellent; Reinforcement protecting material of the present invention and method for reinforcing and protecting implementation and operation are simple, and use the method can make ultimate compression strength be less than 10MPa or the lower crisp powder relics sample of local compressed strength obtains good reinforcement protection.
Further exemplify embodiment below to describe the present invention in detail.Should understand equally; following examples are only used to further illustrate the present invention; can not be interpreted as limiting the scope of the invention, some nonessential improvement that those skilled in the art's foregoing according to the present invention is made and adjustment all belong to protection scope of the present invention., those skilled in the art can do in suitable scope and be selected by explanation herein the temperature that following example is concrete, time, charging capacity etc. are only also examples in OK range,, and do not really want to be defined in the below concrete numerical value of example.
Embodiment 1
A kind ofly reinforce reinforcement protecting material that soluble salt sodium-chlor, calcium chloride etc. cause crisp powder relics to prepare key step as follows:
The hydroxyl endblocked polydimethylsiloxane that adds 5ml molecular weight 700, hydroxyl 4-6%, viscosity 32cst in 50ml tetraethoxy; control 25 ℃ of heating magnetic agitation actuator temperatures; rotating speed 400rpm; after adding magnetic stir bar to stir 24h in liquid, add 0.5ml catalyzer dibutyl tin laurate to stir after 5 minutes, synthetic crisp powder relics reinforcement protecting material.
The protection step of reinforcing the unearthed crisp powder relics relic of Longxian County of Shaanxi shop Qin Mu is as follows:
The method of adopt paper pulp pack, repeatedly implementing is removed the soluble salt of crisp powder relics inside, and the removal that the conductivity value by pulp solution approaches deionization water number judgement soluble salt reaches ideal effect; Adopt ethanol, acetone and other organic solvent to clean historical relic sample surfaces, dry rear surface covers sorbing material cotton gauze, then adopt needle tubing instillation slowly to drip protecting materials, until sorbing material is state of saturation, by processing in the climatic chamber that is positioned over 25 ℃ of temperature, relative humidity 50% after rear crisp powder relics covered with plastic film wraps up, preserve 2 weeks;
After protection, crisp powder relics test result is as follows: 1. adopt the color change value of chromatism of Japanese Minolta CM700D spectrophotometric color measurement instrument test reinforcement protection front and rear surfaces to be less than 2; 2. after adopting Chinese JC2000C contact angle measurement to reinforce, the contact angle of sample surfaces and water is 105.91 °; 3. reinforcement protecting material infiltrates into crisp powder relics sample interior 3mm, and ultimate compression strength improves; 4. the analysis of microcosmic microstructure shows to reinforce the crisp powder particles of rear crisp powder relics sample interior and mutually bonds, and has certain hole between particle; 5. crisp powder relics sample has certain ventilation property, meets " can respiratory " of in humiture changing environment sample hole; 6. analyze crisp powder relics sample under the condition that contains massfraction 2% soluble salt sodium-chlor/calcium chloride; protection effect in the change procedure of preserving 20 ℃ of envrionment temperatures, relative humidity 50% and 96% every 4h circulation, after 78 circulations, crisp powder relics sample does not change.
Embodiment 2
The reinforcement protecting material preparation of crisp powder relics is as embodiment 1;
The protection step of reinforcing crisp powder analog sample is as follows:
After getting Tumulus of Qin Shi Huang, Shaanxi clay 100 orders and sieving, in 700 ℃ of retort furnaces, be fired into the crisp powder particles of ceramic, weigh pottery powder 2.00g, the sample box that employing diameter is 2.5cm is as mould, the dark 6mm of pottery powder sample, reinforcement material 5ml, adopts needle tubing instillation slowly to drip protecting materials, material all infiltrates in pottery powder sample, and the sample after reinforcing is sealed in the climatic chamber that is positioned over 25 ℃ of temperature, relative humidity 50% and preserved 2 weeks;
After protection, crisp powder analog sample test result is as follows: 1. the color change value of chromatism of reinforcement protection front and rear surfaces is less than 2; 2. the apparent porosity 38.35% of sample, volume density 1.35g/cm
3, surface is 100.65 ° with the contact angle of water; 3. reinforcement protecting material infiltrates into sample interior 6mm, and ultimate compression strength improves; 4. microcosmic microstructure analysis shows to reinforce the crisp powder particles of rear sample interior and mutually bonds, and has certain hole between particle; 5. sample has certain ventilation property, meets " can respiratory " of in humiture changing environment sample hole.
Embodiment 3
It is as follows that the reinforcement protecting material of crisp powder relics is prepared key step:
In 50ml tetraethoxy, add the hydroxyl endblocked polydimethylsiloxane that 2.5ml molecular weight 1500, viscosity are 45cst, control 25 ℃ of heating magnetic agitation actuator temperatures, rotating speed 600rpm, after adding magnetic stir bar to stir 24h in liquid, add 0.5ml catalyzer dibutyl tin laurate to stir after 5min, synthetic reinforcement protecting material is stand-by;
The key step of simulation ceramic sample preparation is as follows:
Taking from Tumulus of Qin Shi Huang, Shaanxi clay 100 orders sieves, after 40 ℃ of drying in oven 2h, adopt the brick pressing machine compacting sample piece of just pressure pressure 1MPa, high-pressure 5MPa and at 110 ℃ of drying in oven 24h, object is in order to prevent the too fast volatilization of moisture in sample sintering procedure, to cause sample cracking, is fired into afterwards ultimate compression strength 10Mpa, apparent porosity 37%, volume density 1.60g/cm in 700 ℃ of retort furnaces
3simulation ceramic sample;
The protection step of reinforcing simulation ceramic sample is as follows:
Simulation ceramic sample surfaces covers sorbing material cotton gauze, then adopt banister brush spread coating slowly to add protecting materials, the sample piece of 50mm*50mm*20mm can absorb the protecting materials of 10-20ml, by processing in the climatic chamber that is positioned over 25 ℃ of temperature, relative humidity 50% after rear sample covered with plastic film wraps up, preserves 2 weeks;
After protection, simulation ceramic sample test result is as follows: 1. the color change value of chromatism of reinforcement protection front and rear surfaces is less than 2; 2. the apparent porosity 34% of sample, volume density 1.78g/cm
3, surface is 106.61 ° with the contact angle of water; 3. reinforcement protection sample ultimate compression strength improves; 4. microcosmic microstructure analysis shows to reinforce the crisp powder particles of rear sample interior and mutually bonds, and has certain hole between particle; 5. sample has certain ventilation property, meets " can respiratory " of in humiture changing environment sample hole; 6. analytic sample is under the condition that contains massfraction 3% soluble salt sodium-chlor/calcium chloride, the protection effect in the change procedure of preserving 20 ℃ of envrionment temperatures, relative humidity 50% and 96% every 4h circulation, and after 78 circulations, sample does not change.
Result shows: the crisp powder relics reinforcement material of preparation has certain snappiness, perviousness, the effect that can play bonding, reinforce crisp powder relics, after reinforcing, crisp powder relics surface color changes little, there is certain hydrophobicity, can reduce entering of extraneous water, keep crisp powder relics hole to have certain " can respiratory ", Salt Corrosion is excellent simultaneously.
Industrial applicability
The preparation method of reinforcement material of the present invention and reinforcement means implementation and operation are simple, and use the method can make ultimate compression strength be less than 10MPa or the lower crisp powder relics of local compressed strength obtains good reinforcement protection.
Claims (11)
1. a preparation method for crisp powder relics reinforcement material, is characterized in that, comprising:
Mix tetraethoxy and hydroxyl endblocked polydimethylsiloxane, stir 12～24 hours; And
Gained mixture continues stirring and within 5 minutes, makes above described crisp powder relics reinforcement material under the effect of dibutyltin dilaurate catalyst.
2. preparation method according to claim 1, is characterized in that, described hydroxyl endblocked polydimethylsiloxane is that molecular weight is 400～1500, and hydroxy radical content is 4～6%, the linear reactive polysiloxanes that viscosity is 32～45cst.
3. preparation method according to claim 1 and 2, is characterized in that, the consumption of described hydroxyl endblocked polydimethylsiloxane account for described tetraethoxy volume 5～10%.
4. according to the preparation method described in any one in claim 1～3, it is characterized in that, the consumption of described dibutyltin dilaurate catalyst account for tetraethoxy volume 1%.
5. according to the preparation method described in any one in claim 1～4, it is characterized in that, described stirring adopts magnetic stirring apparatus, coordinates and controls 25 ℃ of temperature, rotating speed 400～600rpm.
6. a reinforcement means for crisp powder relics, is characterized in that, comprising:
Reinforcement material prepared by the preparation method slowly add claim 1～5 on surface coverage has the crisp powder relics of sorbing material in described in any one is until described sorbing material is state of saturation; And
Be transferred in climatic chamber and preserve until described reinforcement material is completely curing.
7. reinforcement means according to claim 6, is characterized in that, described sorbing material is natural or synthetic flexibility fabric.
8. according to the reinforcement means described in claim 6 or 7, it is characterized in that, described relics opposing environment capacity is poor, does not have can support historical relic body intensity, need reinforcement after processing and could preserve for a long time, and its ultimate compression strength is less than 10MPa.
9. according to the reinforcement means described in any one in claim 6～8, it is characterized in that, adopt needle tubing instillation or the banister brush spread coating of not damaging crisp powder surface slowly to add described reinforcement material.
10. according to the reinforcement means described in any one in claim 6～9, it is characterized in that, control 25 ℃ of climatic chamber temperature, relative humidity 50%.
11. according to the reinforcement means described in any one in claim 6～10, it is characterized in that, after consolidation process, described reinforcement material infiltrates into described crisp powder relics inside 3～6mm.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103992729A (en) * | 2014-05-07 | 2014-08-20 | 陕西师范大学 | Reinforcing agent for crisp powder ceramic painted cultural relic |
| CN104163656A (en) * | 2014-07-15 | 2014-11-26 | 南昌大学 | Method for reinforcing carbonate rock stone historical relics |
| CN111499408A (en) * | 2020-04-29 | 2020-08-07 | 同济大学 | Solidified compact carbonate material, solidification method and detection method thereof |
| CN115637104A (en) * | 2022-11-04 | 2023-01-24 | 山东大学 | Preparation method and application of tetraethoxysilane-siloxane-surfactant hybrid material |
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| CN102391013A (en) * | 2011-08-02 | 2012-03-28 | 中国科学院上海硅酸盐研究所 | Method for reinforcing silicate cultural relic |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103992729A (en) * | 2014-05-07 | 2014-08-20 | 陕西师范大学 | Reinforcing agent for crisp powder ceramic painted cultural relic |
| CN103992729B (en) * | 2014-05-07 | 2015-06-17 | 陕西师范大学 | Reinforcing agent for crisp powder ceramic painted cultural relic |
| CN104163656A (en) * | 2014-07-15 | 2014-11-26 | 南昌大学 | Method for reinforcing carbonate rock stone historical relics |
| CN104163656B (en) * | 2014-07-15 | 2016-09-28 | 南昌大学 | A kind of method reinforcing carbonate rock stone cultural artifact |
| CN111499408A (en) * | 2020-04-29 | 2020-08-07 | 同济大学 | Solidified compact carbonate material, solidification method and detection method thereof |
| CN115637104A (en) * | 2022-11-04 | 2023-01-24 | 山东大学 | Preparation method and application of tetraethoxysilane-siloxane-surfactant hybrid material |
| CN115637104B (en) * | 2022-11-04 | 2023-12-22 | 山东大学 | Preparation method and application of ethyl orthosilicate-siloxane-surfactant hybrid material |
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Application publication date: 20140212 |