CN110510985A - A kind of pure inorganic magnesium-based reinforcement material of osmosis type and preparation method and reinforcement means for the reinforcing of sandstones stone cultural artifact - Google Patents
A kind of pure inorganic magnesium-based reinforcement material of osmosis type and preparation method and reinforcement means for the reinforcing of sandstones stone cultural artifact Download PDFInfo
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- CN110510985A CN110510985A CN201910480512.5A CN201910480512A CN110510985A CN 110510985 A CN110510985 A CN 110510985A CN 201910480512 A CN201910480512 A CN 201910480512A CN 110510985 A CN110510985 A CN 110510985A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/30—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing magnesium cements or similar cements
- C04B28/32—Magnesium oxychloride cements, e.g. Sorel cement
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
- C04B2111/00637—Uses not provided for elsewhere in C04B2111/00 as glue or binder for uniting building or structural materials
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Abstract
The invention discloses a kind of pure inorganic magnesium-based reinforcement material of osmosis type reinforced for sandstones stone cultural artifact and preparation method and reinforcement means, its mass percentage composition are as follows: magnesia 5.8%~22.7%, magnesium chloride 8.7%~20.3%, deionized water 9.0%~28.5%, ethyl alcohol 37.2%~74.9%, it is that the dispersion liquid B for preparing the solution A that magnesium chloride and water are prepared for solvent and magnesia with alcohols is formulated according to a certain percentage, it is torn off after being covered on 4~8h of surface with plastic foil after the sandstone of reinforcing liquid infiltration weathering, the aforesaid operations 2-3 times reinforcing that can be realized to weathered sandstone is repeated according to consolidation effect, reinforcement means of the present invention is easy to operate, reinforcement material permeability is good, intensity is high after reinforcing, do not change historical relic original appearance and performance is stablized, right Have broad application prospects in the reinforcing of the serious sandstones stone cultural artifact of weathering.
Description
Technical field
The invention belongs to historical relic's protection fields, and in particular to a kind of osmosis type reinforced for sandstones stone cultural artifact is pure
Inorganic magnesium-based reinforcement material and preparation method and reinforcement means.
Background technique
Outdoor sandstones stone cultural artifact is chronically exposed in natural environment, by violent temperature and humidity variation, air pollution,
The destruction of " dissolution-crystallization " etc. repeatedly factors of microbial growth and soluble salt, surface all gradually generate serious mostly
Weathering Disease.As a result, phenomena such as granular disintegration is presented in cultural artifact surface, layering is flaked and exfoliation, finally loses historical relic
Historical information, artistic value and scientific value etc..Therefore, there is an urgent need to develop the consolidation against weathering material haveing excellent performance.
Reinforcement material currently used for weathered sandstone protection can be divided into organic reinforcement material and inorganic reinforcing material two is big
Class.Wherein, organic reinforcement material mainly has: organo-silicon compound, acrylate copolymer and epoxide resin polymer etc. are several big
Class.Organic reinforcement material fastening strength is high, water resistance is strong, does not change the original appearance of historical relic after reinforcing, but organic reinforcement material is resistance to
Ageing properties are poor, and protection timeliness is limited；Cultural artifact surface forms hydrophobic layer after the processing of organic reinforcement material, in natural environment
The phenomenon that " organic protection layer-inorganic bulk " interface peel can be generated under destroying, the poor compatibility with historical relic ontology may be right
Historical relic generates protectiveness and destroys.Inorganic reinforcing material can be divided into according to its effective component: calcium base, barium base and silicon substrate etc..It is inorganic to add
Gu the advantages of material is that performance is stable, weatherability is strong, but mechanical strength is not apparent after the reinforcing of some inorganic reinforcing materials
It improves；Most inorganic reinforcing material is indissoluble or micro-soluble material, limited penetration depth, these unfavorable factors limit inorganic reinforcing
Application of the material in historical relic's protection.But inorganic material it is strong, more compatible with historical relic ontology as a kind of weatherability, can
Lasting reinforcement material is the trend of future development.
According to the specific requirement in China's conservation of historic landmarks and sites criterion to protection materials, protection materials should meet following item
Part: 1. there is certain penetration depth, and the reinforcing liquid of unit mass answers reinforcing historical relic ontology as much as possible, that is, reinforces effect
Rate is high；2. protection materials cannot change historical relic original appearance, i.e., the color difference that reinforcing liquid reinforces front and back will be in human eye recognizable set
(△E*<5)；3. have certain fastening strength, fastening strength can not it is excessively high can not be too low.
To meet above-mentioned condition and solve the problems, such as the weathering of sandstone, the present invention proposes a kind of to meet historical relic's protection requirement
Liquid and reinforcement means are reinforced by the pure inorganic magnesium-based of the osmosis type of dispersing agent of alcohol.Present invention exploration is formed in the sandstone of weathering
With the compound of argillaceous cement identity function, which can be with remaining particle in sandstone ontology by reinforcing consolidating for liquid
Change reaction to combine closely, to realize the purpose of reinforcing.
Summary of the invention
For the technical problems to be solved by the invention, the present invention provides a kind of fastening strength height, good penetrability, does not change
The pure inorganic magnesium-based of popular form of narrative literature flourishing in the Tang Dynasty object original appearance reinforces liquid, preparation method and reinforcement means, and the present invention is to come by the following technical programs in fact
Existing:
The invention discloses a kind of pure inorganic magnesium-baseds of osmosis type reinforced for weathered sandstone to reinforce liquid, by following quality
The raw material of per distribution ratio forms:
As a further improvement, raw material magnesia of the present invention is pre-processed: by magnesia in drying
Dry 3h under the conditions of 100 DEG C, crosses the sieve of 180 mesh, prevents magnesia from agglomerating in case after taking-up, guarantees magnesium oxide particle less than 80 μ
M is easily dispersed.
The invention also discloses the preparation sides that a kind of pure inorganic magnesium-based of osmosis type reinforced for weathered sandstone reinforces liquid
Method, steps are as follows:
It 1) is, MgCl according to molar ratio by deionized water2·6H2O:H2O=1:(10~20) ratio be added MgCl2·
6H2Magnesium chloride solution ie in solution A is obtained in O；
2) be, 1:(2~5 according to mass ratio by the magnesia weighed up and dispersing agent ethyl alcohol) mixing, be then placed in ultrasound
10~15min of ultrasound, makes magnesia be dispersed in ie in solution B in alcohol solvent in cleaning device；
It 3) by solution A and solution B according to molar ratio is MgCl when, using2·6H2O:MgO=1:(3~7) ratio will
Solution A is slowly added in solution B and is stirred continuously obtain permeable pure inorganic magnesium-based reinforcing liquid, reinforces under the ratio
The consolidation effect of liquid is totally in best.
As a further improvement, penetration reinforcement liquid of the present invention is just to mix solution A and B when using.
As a further improvement, in step 3) of the present invention, before penetration reinforcement by solution A ultrasonic disperse 10~
15min adds solution B after solution A is uniformly dispersed.
The invention discloses the reinforcement means that a kind of pure inorganic magnesium-based of the osmosis type reinforced for weathered sandstone reinforces liquid,
Penetration reinforcement is carried out to loose sandstone using the method for drop infiltration or injection, is drawn add with rubber head dropper or syringe first
Solid-liquid is added dropwise according to the speed of 0.5~1.5mL/min on the surface of weathered sandstone, and solid-liquid to be added uses modeling after fully penetrating into rock
Material film is torn off after being covered on surface 4-8h, repeats 2~3 reinforcings that can be realized to weathered sandstone of aforesaid operations.
Beneficial effects of the present invention are as follows:
Magnesia, which need to dry the reason of sieving, in pretreatment of raw material of the present invention is: magnesia is in the process for preparing and placing
Unavoidably there is caking phenomenon, magnesium oxide particle is big after agglomeration, it is not easy to disperse.
For the present invention with the screen filtration magnesia of 180 mesh in pretreatment of raw material, the purpose is to filter off the oxidation of bulky grain
Magnesium prevents plus solid-liquid reaction is insufficient, influences consolidation effect, prevents bulky grain to be deposited on cultural artifact surface blocking and reinforce liquid and penetrate into and leads to
It road and stays in cultural artifact surface the apparent colour of historical relic is had an impact.
The present invention makees dispersing agent with ethyl alcohol in reinforcing liquid preparation, the reason is that ethyl alcohol is volatile solvent, is reinforcing liquid
It will be slow volatilization during cured, destruction will not be generated to historical relic, and the ethyl alcohol to volatilize does not pollute the environment, be a kind of
More satisfactory dispersing agent.Ethyl alcohol not with add solid-liquid reaction, the consolidation effect for reinforcing liquid will not be destroyed, reinforce liquid through ethyl alcohol point
Penetration depth obviously increases after dissipating.The effect of ethyl alcohol is that dilution reinforces liquid and improves the penetration depth for reinforcing liquid.
The present invention is covered after penetration reinforcement operates with plastic foil, be in order to prevent ethyl alcohol in temperature compared with Gao Shihui
It sends out too fast, forces ethyl alcohol with liquid is reinforced along the hole endosmosis of weathered sandstone, the purpose is to improve the infiltration for reinforcing liquid
Depth enhances consolidation effect.
The present invention is using ethyl alcohol as the pure inorganic with magnesia, magnesium chloride and water osmosis type as main component of dispersing agent
Magnesium-based reinforces liquid, reinforces liquid and penetrates into sandstone pores, as the solvent evaporates, reinforces liquid and is cured reaction, generate needle-shaped knot
Crystalline substance combines closely sandstone particle, to realize the purpose for reinforcing sandrock；The present invention reinforces liquid to improve
Penetration depth using not with add solid-liquid reaction ethyl alcohol be dispersing agent；After the present invention reinforces liquid reinforcing sandstone, the machinery of sandstone is strong
Degree improves, and reinforces inanimate matter historical relic, reinforcement material and historical relic ontology good compatibility with inorganic material, ageing-resistant soaking-resistant is green
Colour circle is protected, and is a kind of reinforcement material having wide application prospects.
Detailed description of the invention
Fig. 1 is microscopic appearance figure (a) × 5000 for reinforcing section after liquid solidifies；
Fig. 2 is microscopic appearance figure (b) × 10000 for reinforcing section after liquid solidifies；
Fig. 3 is microscopic appearance figure (c) × 500 for reinforcing liquid and reinforcing sandstone particle；
Fig. 4 is microscopic appearance figure (d) × 1500 for reinforcing liquid and reinforcing sandstone particle.
Specific embodiment
The invention discloses a kind of pure inorganic magnesium-baseds of osmosis type reinforced for weathered sandstone to reinforce liquid, by following quality
The raw material of per distribution ratio forms:
Raw material magnesia is pre-processed: magnesia being dried to 3h in drying box, after taking-up under the conditions of 100 DEG C
The sieve of 180 mesh is crossed, the magnesium oxide particle is less than 80 μm.
The pure inorganic magnesium-based of osmosis type reinforced above for weathered sandstone reinforces the preparation method of liquid, which is characterized in that step
It is rapid as follows:
It 1) is, MgCl according to molar ratio by deionized water2·6H2O:H2O=1:(10~20) ratio be added MgCl2·
6H2Magnesium chloride solution ie in solution A is obtained in O；
2) be, 1:(2~5 according to mass ratio by the magnesia weighed up and dispersing agent ethyl alcohol) mixing, be then placed in ultrasound
10~15min of ultrasound, makes magnesia be dispersed in ie in solution B in alcohol solvent in cleaning device；
It 3) by solution A and solution B according to molar ratio is MgCl when, using2·6H2O:MgO=1:(3~7) ratio will
Solution A is slowly added in solution B and is stirred continuously obtain permeable pure inorganic magnesium-based reinforcing liquid, will be molten before penetration reinforcement
Liquid A 10~15min of ultrasonic disperse, adds solution B after solution A is uniformly dispersed.
Penetration reinforcement liquid is just to mix solution A and B when using.
The invention also discloses the reinforcing sides that a kind of pure inorganic magnesium-based of osmosis type reinforced for weathered sandstone reinforces liquid
Method, is seeped using drop or the method for injection carries out penetration reinforcement to loose sandstone, is drawn first with rubber head dropper or syringe
Liquid is reinforced, is added dropwise according to the speed of 0.5~1.5mL/min on the surface of weathered sandstone, solid-liquid to be added is used after fully penetrating into rock
Plastic foil is torn off after being covered on surface 4-8h, repeats 2~3 reinforcings that can be realized to weathered sandstone of aforesaid operations.
Technical solution of the present invention is further described below by specific embodiment:
Embodiment 1
One, the preparation of liquid is reinforced
Weigh 3.6g H2O and 2.033g MgCl2·6H2It is solution A that O, which is mixed to get magnesium chloride solution,；Weigh 2gMgO
It is uniformly mixed with 10g dehydrated alcohol, then ultrasound 10min, being dispersed in magnesium oxide powder is solution in alcohol solvent
Then solution A is added stirring in solution B and reconciled to the reinforcing liquid that uniformly as can be used for penetration reinforcement by B.Osmosis type is reinforced
Liquid uses in 1h.
Two, liquid performance test is reinforced
(1) penetration depth, strengthening quality and acetes chinensis reinforce liquid made from rubber head dropper absorption 1g, according to 1mL/
The speed of min instills in loose silica sand, after solid-liquid to be added is fully cured in sand, takes out the part of reinforcing, uses vernier respectively
The gentle chromascope in slide calliper rule, day tests its penetration depth, strengthening quality and color difference.Measuring its penetration depth is 34.52mm, is reinforced
Quality is 7.604g, after reinforcing with the color difference of ontology be 3.4.
(2) compression strength detection stirs evenly the effective component for reinforcing liquid and silica sand according to the ratio that mass ratio is 1:4
Compacting in filling cuboid sample model (20mm × 20mm × 20mm) afterwards.After 2 days, sample is taken out from metal die.In
It is conserved in the environment of 25 ± 10 DEG C of temperature, relative humidity 60 ± 20%.Microcomputer controlled electronic universal testing machine is used after a week
The compression strength of test simulation sample block, record sample destroy when peak load, calculate test block pressure resistance intensity be 12.7MPa.
(3) water resistance test will be simulated after sample block impregnates 15 days in water and be taken out, and compared with before water immersion, surface is without bright
Show visible variation.The water that surface is sucked with filter paper is put into 105 DEG C of drying box for 24 hours, is cooled to room temperature after taking-up, claims
Amount, compared with before immersion, mass loss rate 4.72%, less than 5%, and testing its compression strength is 10.6MPa.
(4) it is to reinforce that Morphology analysis Fig. 1, which is the microscopic appearance figure (a) × 5000, Fig. 2 in section after reinforcing liquid solidifies,
After liquid solidifies the microscopic appearance figure (b) × 10000, Fig. 3 in section be reinforce liquid reinforce sandstone particle microscopic appearance figure (c) ×
500, Fig. 4 be microscopic appearance figure (d) × 1500 for reinforcing liquid and reinforcing sandstone particle.Prepared mixed solution 30ml is taken, is stood
Conserved one week in the environment of 25 ± 10 DEG C of temperature, relative humidity 60 ± 20%, will solidification sample block cutting, exposure section with into
Row imaging as can be seen from the figure reinforces compact structure after liquid solidification referring to Fig. 1 and 2, shows reaction sufficiently, intensity is high.From
It can be seen that there is many 5 acicular crystals of phase in stomata in figure, after the presence of this bubble and acicular crystal ensure that sandstone is reinforced
Gas permeability.Fig. 3 and 4 is to reinforce in the gap that liquid is filled between sand grains and sand grains after solidifying in sandstone, while reinforcing liquid
With sandstone particle remaining in sandstone ontology by reinforce liquid curing reaction combine closely, acicular crystal there are energy
It is enough inserted into the small spaces inside sandstone, there is very high intensity, can be realized the reinforcing to sandrock.
Embodiment 2
One, the preparation of liquid is reinforced
Weigh 3.24g H2O and 2.033g MgCl2·6H2It is solution A that O, which is mixed to get magnesium chloride solution,；It weighs
2.8gMgO and 12g dehydrated alcohol is uniformly mixed, and then ultrasound 10min, is dispersed in magnesium oxide powder in alcohol solvent
Then solution A is added stirring in solution B and reconciled to the reinforcing liquid that uniformly as can be used for penetration reinforcement by as solution B.It seeps
Saturating type is reinforced liquid and is used in 1h.
Two, liquid performance test is reinforced
(1) penetration depth, strengthening quality and acetes chinensis reinforce liquid made from rubber head dropper absorption 1g, according to 1mL/
The speed of min instills in loose silica sand, after solid-liquid to be added is fully cured in sand, takes out the part of reinforcing, uses vernier respectively
The gentle chromascope in slide calliper rule, day tests its penetration depth, strengthening quality and color difference.Measuring its penetration depth is 30.74mm, is reinforced
Quality is 7.307g, after reinforcing with the color difference of ontology be 4.7.
(2) fastening strength detection stirs evenly the effective component for reinforcing liquid and silica sand according to the ratio that mass ratio is 1:4
Compacting in filling cuboid sample model (20mm × 20mm × 20mm) afterwards.After 2 days, sample is taken out from metal die.In
It is conserved in the environment of 25 ± 10 DEG C of temperature, relative humidity 60 ± 20%.Microcomputer controlled electronic universal testing machine is used after a week
The compression strength of test simulation sample block, record sample destroy when peak load, calculate test block pressure resistance intensity be 10.3MPa.
(3) water resistance test will be simulated after sample block impregnates 15 days in water and be taken out, and compared with before water immersion, surface is without bright
Show visible variation.The water that surface is sucked with filter paper is put into 105 DEG C of drying box for 24 hours, is cooled to room temperature after taking-up, claims
Amount, compared with before immersion, mass change 4.54%, less than 5%, and testing its compression strength is 7.5MPa.
Embodiment 3
With embodiment 1, magnesia is only changed to the magnesia for making to handle without dried and screened, other steps and implementation
Example 1 is identical.Liquid is reinforced made from rubber head dropper absorption 1g, instills in loose silica sand, finds according to the speed of 1mL/min
There is the magnesia of bulky grain not penetrate into inside silica sand, there are white powder deposition, color difference 8.9 in surface.Illustrate to magnesium oxide powder
Sample pre-treatments are necessary.
Embodiment 4
With embodiment 1, the amount that ethyl alcohol is added only is changed to 15g, other steps are same as Example 1.It instills loosely
Measuring in silica sand and reinforcing the penetration depth of liquid is 34.34mm, is declined than embodiment 1, illustrates that the mass fraction of ethyl alcohol is more than
The penetration depth of 74.9% post-reinforcing liquid not will increase.
Embodiment 5
With embodiment 2, covered after only reinforcing with plastic foil, penetration depth increases than embodiment 1, illustrates plastics
Film covering has positive effect to penetration depth is promoted.
Embodiment 6
With embodiment 2, the amount that water is added only is increased into 4.5g, other steps are same as Example 2.Mould obtained
The compressive strength rate embodiment 1 of quasi- sample block is declined, and illustrates that excessive water is unfavorable for reinforcing the solidification of liquid, the dosage of water is not
It is preferably excessive.
Embodiment 7
With embodiment 2, the magnesia amount of being put into, which will only be added, increases to 4.4g, other steps are identical as embodiment 2.It surveys
Its penetration depth is 25.68mm, with the color difference of ontology be 11.9 after reinforcing, illustrate the content when magnesia greater than 22.7%
When, reinforcing liquid cannot penetrate into sandstone well and be affected to the sandstone apparent colour after solidification.
The above enumerated are only specific embodiments of the present invention for finally, it should also be noted that.Obviously, the present invention is unlimited
In above embodiments, acceptable there are many deformations.Those skilled in the art can directly lead from present disclosure
Out or all deformations for associating, it is considered as protection scope of the present invention.
Claims (6)
1. a kind of pure inorganic magnesium-based of osmosis type reinforced for weathered sandstone reinforces liquid, which is characterized in that by following quality percentages
The raw material of proportion forms:
2. the pure inorganic magnesium-based of osmosis type reinforced as described in claim 1 for weathered sandstone reinforces liquid, which is characterized in that institute
The raw material magnesia stated is pre-processed: magnesia being dried under the conditions of 100 DEG C to 3h in drying box, 180 are crossed after taking-up
Purpose sieve, the magnesium oxide particle is less than 80 μm.
3. the preparation side that a kind of pure inorganic magnesium-based of osmosis type reinforced as described in claim 1 for weathered sandstone reinforces liquid
Method, which is characterized in that steps are as follows:
It 1) is, MgCl according to molar ratio by deionized water2·6H2O:H2O=1:(10~20) ratio be added MgCl2·6H2In O
Obtain magnesium chloride solution ie in solution A；
2) be, 1:(2~5 according to mass ratio by the magnesia weighed up and dispersing agent ethyl alcohol) mixing, be then placed in ultrasonic cleaning
10~15min of ultrasound, makes magnesia be dispersed in ie in solution B in alcohol solvent in instrument；
It 3) by solution A and solution B according to molar ratio is MgCl when, using2·6H2O:MgO=1:(3~7) ratio by solution A
It is slowly added in solution B and is stirred continuously obtain permeable pure inorganic magnesium-based reinforcing liquid.
4. the pure inorganic magnesium-based of osmosis type reinforced as claimed in claim 3 for weathered sandstone reinforces the preparation method of liquid,
It is characterized in that, the penetration reinforcement liquid is just to mix solution A and B when using.
5. the osmosis type pure inorganic magnesium-based as described in claim 1 reinforced for weathered sandstone according to claim 3
Reinforce liquid preparation method, which is characterized in that in the step 3), before penetration reinforcement by solution A ultrasonic disperse 10~
15min adds solution B after solution A is uniformly dispersed.
6. the reinforcing side that a kind of pure inorganic magnesium-based of osmosis type reinforced as described in claim 1 for weathered sandstone reinforces liquid
Method, which is characterized in that seeped using drop or the method for injection carry out penetration reinforcement to loose sandstone, first with rubber head dropper or
Syringe, which is drawn, reinforces liquid, is added dropwise according to the speed of 0.5~1.5mL/min on the surface of weathered sandstone, solid-liquid to be added seeps completely
Enter and torn off after being covered on surface 4-8h with plastic foil after rock, repeats aforesaid operations 2~3 times and can be realized to add weathered sandstone
Gu.
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| CN201910480512.5A CN110510985B (en) | 2019-06-04 | 2019-06-04 | Permeable pure inorganic magnesium-based reinforcing material for reinforcing sandstone stone cultural relics, and preparation method and reinforcing method thereof |
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| CN201910480512.5A CN110510985B (en) | 2019-06-04 | 2019-06-04 | Permeable pure inorganic magnesium-based reinforcing material for reinforcing sandstone stone cultural relics, and preparation method and reinforcing method thereof |
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| CN113087545A (en) * | 2021-04-02 | 2021-07-09 | 浙江大学 | Pure inorganic strengthening-moss removing compound agent for protecting weathered stone cultural relics and preparation method thereof |
| CN113563806A (en) * | 2021-08-09 | 2021-10-29 | 浙江大学 | Inorganic magnesium-based adhesive for bonding and grouting fractured stone cultural relics and preparation method thereof |
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| CN113563806A (en) * | 2021-08-09 | 2021-10-29 | 浙江大学 | Inorganic magnesium-based adhesive for bonding and grouting fractured stone cultural relics and preparation method thereof |
| CN113563806B (en) * | 2021-08-09 | 2022-04-12 | 浙江大学 | Inorganic magnesium-based adhesive for bonding and grouting fractured stone cultural relics and preparation method thereof |
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| CN110510985B (en) | 2021-01-05 |
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