CN109704662A - A kind of nano-silicon nitride enhancing cement-based material and preparation method thereof - Google Patents
A kind of nano-silicon nitride enhancing cement-based material and preparation method thereof Download PDFInfo
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Abstract
The present invention provides a kind of nano-silicon nitride enhancing cement-based material and preparation method thereof, mainly includes three steps: being the heat treatment of nano silicon nitride silicon materials first, nano silicon nitride silicon materials are heat-treated；Then dispersant with high efficiency is added in the nano silicon nitride silicon materials after heat treatment and is prepared into nano silicon nitride silicon suspension；Nano silicon nitride silicon suspension is finally added to agitator for cement mortar to the stirring for carrying out certain way, is prepared into nanometer enhancing silicon nitride cement-based material.Nanometer prepared by the present invention enhances silicon nitride cement-based material, preparation process is simple, it is easy to operate, after nano-silicon nitride is added, improve the microstructure of cement slurry, reduce porosity, the defects of reducing hole present in cement slurry and crackle, dense micro-structure is improved, substantially improves the mechanical property of cement slurry, in 0.16% incorporation of nano-silicon nitride, 28d compression strength improves 24.6%, and 28 days flexural strengths improve 19.8%.
Description
Technical field
The invention belongs to cement-based material technical fields, and in particular to a kind of nano-silicon nitride enhancing cement-based material and its
Preparation method.
Background technique
Cement-based material has the characteristics that uniqueness, such as bonding capacity is good, intensity is high, durability is good, therefore cement is being built
It is always one of most widely used construction material in material industry.But since the physical characteristic of cement itself determines it with very prominent
Out the shortcomings that.Due to the contraction of cement in the curing process, so that the defects of there are a large amount of hole, crack, crackles in cement,
And from great, easy embrittlement substantially reduces its endurance quality.
The defects of physical characteristic and its application in view of cement, in order to have cement applications in building trade more preferably
Performance, improve its intensity and durability, using nano material cement be modified and to be studied as current scientific research scholars
Hot spot it is expected that the physics filling effect of nano material can improve the microstructure of cement, and then improves cement-based material
Mechanical property improves durability, and there is presently no a kind of methods that simplicity is easily operated, has after enabling to nano material to be added
Effect improves the mechanical property of cement-based material.
Accordingly, it is desirable to provide a kind of be directed to the insufficient improved technology scheme of the above-mentioned prior art.
Summary of the invention
The purpose of the present invention is to provide a kind of nano-silicon nitride enhancing cement-based materials and preparation method thereof, using nanometer
Silicon nitride is added in cement-based material, to improve the microstructure of cement, porosity is reduced, to improve cement-based material
Mechanical property.
To achieve the goals above, the invention provides the following technical scheme:
A kind of preparation method of nano-silicon nitride enhancing cement-based material, the preparation method of the cement-based material include with
Lower step:
The heat treatment of S1, nano-silicon nitride
Nano-silicon nitride is contained up in heatproof container, baking oven is put into and is heated, makes nano silicon nitride silicon face
Impurity overflows, and takes out nano-silicon nitride after heat treatment；
The decentralized processing of S2, nano-silicon nitride
Water is added into container, then the nano-silicon nitride after heat treatment is put into container, then is added and divides into container
Powder after addition, forms the suspension of nano-silicon nitride；Nano silicon nitride silicon suspension is subjected to mechanical stirring, machinery stirs
Ultrasonic disperse is carried out after mixing；
The preparation of S3, cement-based material
By ultrasonic disperse in step S2, treated that nano silicon nitride silicon suspension is added into blender, then to blender
Middle addition water and cement, obtain cement-based material mixed liquor, are stirred to cement-based material mixed liquor, obtain nano-silicon nitride
Enhance cement-based material.
In the preparation method of nano-silicon nitride as described above enhancing cement-based material, it is preferable that nanometer nitrogen in step S1
The heating temperature of SiClx heat treatment is 325 DEG C~375 DEG C, and heating time is 30min~120min.
In the preparation method of nano-silicon nitride as described above enhancing cement-based material, it is preferable that disperse described in step S2
Agent is polycarboxylic acids dehydragent；
Preferably, the additional amount of the dispersing agent accounts for the 0.01%~0.5% of cement quality.
In the preparation method of nano-silicon nitride as described above enhancing cement-based material, it is preferable that nano silicon nitride in step S3
The additional amount of silicon suspension is no more than the 2% of nano-silicon nitride enhancing cement-based material；
Preferably, the additional amount of nano silicon nitride silicon suspension accounts for nano-silicon nitride enhancing cement-based material in step S3
0.01%~0.2%.
In the preparation method of nano-silicon nitride as described above enhancing cement-based material, it is preferable that by nanometer nitrogen in step S2
SiClx suspension carries out the churned mechanically time as 2min~7min, and the time of ultrasonic disperse is no less than 30min.
In the preparation method of nano-silicon nitride as described above enhancing cement-based material, it is preferable that the nano-silicon nitride is outstanding
It is 500r/min~1000r/min that supernatant liquid, which carries out churned mechanically revolving speed,.
In the preparation method of nano-silicon nitride as described above enhancing cement-based material, it is preferable that be added in step S3 to institute
The ratio of mud for stating the water and cement in blender is 0.28~0.40.
In the preparation method of nano-silicon nitride as described above enhancing cement-based material, it is preferable that cement base in step S3
The agitating mode that material mixed liquor is stirred is first to mix slowly 120s, and revolving speed is 135r/min~145r/min, is then stopped
15s is only stirred, then quickly stirring 120s, revolving speed are 275r/min~295r/min, are then stopped.
In the preparation method of nano-silicon nitride as described above enhancing cement-based material, it is preferable that nano silicon nitride in step S1
The average particle size of silicon is 10nm~30nm.
A kind of nano-silicon nitride enhancing cement-based material of the preparation method preparation of nano-silicon nitride enhancing cement-based material.
Compared with the immediate prior art, technical solution provided by the invention has following excellent effect:
Nano-silicon nitride provided by the invention enhances cement-based material, is after being handled for nano-silicon nitride, then
It is added in cement grout in certain proportion, and the materials such as additive is added, to improve the physical mechanics of cement-based material
Performance and durability；Nano-silicon nitride of the invention enhances cement-based material, porosity is reduced, so that microstructure is more stepped up
It is close, to improve the mechanical property of cement slurry；In 0.16% incorporation of nano-silicon nitride, 28d compression strength is improved
24.6%, and 28 days flexural strengths improve 19.8%.
Detailed description of the invention
The accompanying drawings constituting a part of this application is used to provide further understanding of the present invention, and of the invention shows
Examples and descriptions thereof are used to explain the present invention for meaning property, does not constitute improper limitations of the present invention.Wherein:
Fig. 1 is the compression strength comparison diagram of each age of the embodiment of the present invention 1 and reference examples 1；
Fig. 2 is the compression strength comparison diagram of each age of the embodiment of the present invention 1 and reference examples 2；
Fig. 3 is the compression strength comparison diagram of each age of the embodiment of the present invention 1 and reference examples 3；
Fig. 4 is the flexural strength comparison diagram of each age of the embodiment of the present invention 1 and reference examples 1；
Fig. 5 is the flexural strength comparison diagram of each age of the embodiment of the present invention 1 and reference examples 2；
Fig. 6 is the flexural strength comparison diagram of each age of the embodiment of the present invention 1 and reference examples 3.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiments of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is general
Logical technical staff's every other embodiment obtained, shall fall within the protection scope of the present invention.
The present invention will be described in detail below with reference to the accompanying drawings and embodiments.It should be noted that in the feelings not conflicted
Under condition, the feature in embodiment and embodiment in the present invention be can be combined with each other.
The preparation method of nano-silicon nitride enhancing cement-based material provided by the invention, mainly includes three steps: first
It is the heat treatment of nano silicon nitride silicon materials, nano silicon nitride silicon materials is carried out to the heat treatment of certain temperature and time；It then will be hot
Treated, and nano silicon nitride silicon materials addition dispersant with high efficiency is prepared into nano silicon nitride silicon suspension；Finally nano-silicon nitride is hanged
The stirring for carrying out certain way is added to agitator for cement mortar in supernatant liquid, is prepared into nanometer enhancing silicon nitride cement-based material.This
The nanometer of invention preparation enhances silicon nitride cement-based material, and preparation process is simple, easy to operate, after nano-silicon nitride is added, improves
The microstructure of cement slurry the defects of reduce porosity, reduce hole present in cement slurry and crackle, improves
Dense micro-structure, substantially improves the mechanical property of cement slurry, and 28d is anti-in 0.16% incorporation of nano-silicon nitride
Compressive Strength improves 24.6%, and 28 days flexural strengths improve 19.8%.
Nano-silicon nitride has the advantage that compared with similar nano material firstly, nano-silicon nitride performance is stablized, in water
Physics filling effect is mainly played in cement-based material, improves the consistency of cement-based material；Secondly, nano-silicon nitride hardness itself
It is very high, it is mostly used in the products such as ceramics, is added to the intensity and hardness that can be improved cement-based material in cement-based material；Most
Afterwards, since nano-silicon nitride intensity itself is high, it is added to the resisting chloride ion penetration infiltration that can be improved cement-based material in cement-based material
Saturating ability.
A kind of preparation method of nano-silicon nitride enhancing cement-based material provided by the invention, comprising the following steps:
The heat treatment of S1, nano-silicon nitride
Nano-silicon nitride is contained up in heatproof container, baking oven is put into and is heated, makes nano silicon nitride silicon face
Impurity overflows, and takes out nano-silicon nitride after heat treatment；
It preferably, is 325 DEG C~375 DEG C (such as 330 to the heating temperature of nano-silicon nitride heat treatment in step S1
DEG C, 335 DEG C, 340 DEG C, 345 DEG C, 350 DEG C, 355 DEG C, 360 DEG C, 365 DEG C, 370 DEG C, 375 DEG C), heating time be 30min~
120min (such as 40min, 50min, 60min, 70min, 80min, 90min, 100min, 110min).
The decentralized processing of S2, nano-silicon nitride
Water is added into container, then the nano-silicon nitride after heat treatment is put into container, then is added and divides into container
Powder after addition, forms the suspension of nano-silicon nitride, and nano silicon nitride silicon suspension is carried out mechanical stirring, stirring knot
Ultrasonic disperse is carried out after beam.
Preferably, nano silicon nitride silicon suspension carry out churned mechanically revolving speed be 500r/min~1000r/min (such as
550r/min、600r/min、650r/min)。
Preferably, dispersing agent is polycarboxylic acids dehydragent in step S2；Preferably, the additional amount of dispersing agent accounts for cement quality
0.01%~0.5% (such as 0.05%, 0.08%, 0.1%, 0.15%, 0.2%, 0.25%, 0.3%, 0.35%,
0.4%, 0.45%, 0.5%).
Preferably, in step S2 by nano silicon nitride silicon suspension carry out churned mechanically time be 2min~7min (such as
3min, 4min, 5min, 6min), the time of ultrasonic disperse is not less than 30min.
Preferably, the average particle size of nano-silicon nitride be 10nm~30nm (such as 12nm, 14nm, 16nm, 18nm,
20nm, 22nm, 24nm, 26nm, 28nm, 30nm), granularity is small, is evenly distributed after decentralized processing, large specific surface area, surface
Active height is distributed in cement-based material the reinforcing effect that can greatly improve cement-based material, and the addition of nano-silicon nitride makes
The defects of cement slurry microstructure is finer and close, reduces porosity, reduces hole present in cement slurry and crackle, because
This makes the intensity of cement-based material make moderate progress.
The preparation of S3, cement-based material
Nano silicon nitride silicon suspension after decentralized processing in step S2 is added into blender, is then added into blender
Enter water and cement, obtain cement-based material mixed liquor, cement-based material mixed liquor is stirred, obtains nano-silicon nitride enhancing
Cement-based material.
Preferably, the additional amount of nano silicon nitride silicon suspension is no more than nano-silicon nitride enhancing cement-based material in step S3
2%；Preferably, the additional amount of nano silicon nitride silicon suspension accounts for nano-silicon nitride enhancing cement-based material in step S3
0.01%~0.2% (such as 0.02%, 0.03%, 0.04%, 0.05%, 0.06%, 0.07%, 0.08%, 0.09%,
0.1%, 0.12%, 0.13%, 0.14%, 0.15%, 0.16%, 0.17%, 0.18%, 0.19%, 0.2%)；Further preferably
Ground, the additional amount of nano silicon nitride silicon suspension accounts for the 0.16% of nano-silicon nitride enhancing cement-based material in step S3.
Preferably, the ratio of mud that water and cement into blender are added in step S3 be 0.28~0.40 (such as 0.29,
0.3、0.31、0.32、0.33、0.34、0.35、0.36、0.37、0.38、0.39)。
It preferably, is first to mix slowly 120s to the agitating mode that cement-based material mixed liquor is stirred in step S3,
Revolving speed be 135r/min~145r/min (such as 136r/min, 137r/min, 138r/min, 139r/min, 140r/min,
141r/min, 142r/min, 143r/min, 144r/min), then stop stirring 15s, then quickly stirring 120s, revolving speed are
275r/min~295r/min (such as 276r/min, 277r/min, 278r/min, 279r/min, 280r/min, 281r/min,
282r/min、283r/min、284r/min、285r/min、286r/min、287r/min、288r/min、289r/min、290r/
Min, 291r/min, 292r/min, 293r/min, 294r/min), then stop.
Embodiment 1
A kind of preparation method of nano-silicon nitride enhancing cement-based material provided by the invention, first progress nano-silicon nitride
Processing: hold nano silicon nitride silicon materials with corundum crucible, nano-silicon nitride quality is 5g, average grain diameter 20nm, by nanometer
Silicon carbide is put into baking oven, and the heat treatment of 30min is carried out under the conditions of 350 DEG C, and nano silicon nitride silicon raw material was fabricating
Cheng Zhong, surface can contain ammonium chloride, the ammonium chloride on nano-silicon nitride surface can be made to overflow by heat treatment.
A kind of nano-silicon nitride provided by the invention enhances the preparation method of cement-based material, includes on the basis of above-mentioned
Following steps:
Step 1: the decentralized processing of nano-silicon nitride
Water 72g is weighed, the nano-silicon nitride 0.384g after heat treatment is added adds polycarboxylic acids dehydragent, water-reducing agent
Additional amount is 0.096g, and it is 0.04% that water-reducing agent, which accounts for cement quality ratio,；The machinery for carrying out 2min after being poured into beaker in order stirs
It mixes, revolving speed 1000r/min；Then the ultrasonic disperse that 30min is carried out under the power condition of 250w, it is outstanding to obtain nano-silicon nitride
Supernatant liquid.
Step 2: the preparation of nano-silicon nitride cement-based material slurries
It is 0.3 that water and the cement addition proportion ratio of mud are controlled when preparing nano-silicon nitride cement-based material, net in cement
Slurry blender in sequentially add nano silicon nitride silicon suspension 72.480g, reference cement 240g is then stirred mixed liquor, slowly
Speed stirring 120s, revolving speed 140r/min, stop mixing 15s, then quickly then stirring 120s, revolving speed 285r/min shut down, obtain
To nano-silicon nitride cement-based material slurries.
It is 0.16% that nano-silicon nitride incorporation, which accounts for the ratio of cement-based material, in the present embodiment.
Step 3: preparing nano-silicon nitride cement-based material test specimen
By the nano-silicon nitride cement-based material slurries prepared in 20mm × 20mm × 20mm die for molding, vibrating
1min is vibrated on platform, preservative film is sticked after its condensation and is put in thermostatic chamber, and rear demoulding, is placed in 20 DEG C, the wet feeding room 95%RH for 24 hours
In conserved, obtain nano-silicon nitride cement base slurry.
Then respectively test the present embodiment in nano-silicon nitride cement base slurry 1d, 3d, 7d, 28d compression strength,
And test the microstructure of the nano-silicon nitride cement base slurry under corresponding number of days respectively with scanning electron microscope.
Strength test results are as follows: 1d compression strength is 33.640Mpa；3d compression strength is 54.923Mpa；7d compression strength
For 65.256MPa；28 days compression strength is 101.172Mpa.
Microstructure analysis result: to the nano-silicon nitride cement base slurry under 1d, 3d, 7d, 28d in the present embodiment into
Row Micro-Structure Analysis finds compact structure, is free of obvious bubble, and without apparent crackle.
Embodiment 2
It is 325 DEG C, when heating that step 1, which is changed to the heating temperature of nano-silicon nitride heat treatment, in the present embodiment
Between be 50min, the average particle size of nano-silicon nitride is 30nm, the nano-silicon nitride 0.048g after heat treatment is added, diminishing
Agent additional amount is 0.24g, and it is 0.1% that water-reducing agent, which accounts for cement quality ratio,；And nano silicon nitride silicon suspension is added in step 2
72.288g, reference cement 240g, it is 0.02% that nano-silicon nitride incorporation, which accounts for the ratio of cement-based material, in the present embodiment,
His method and step is same as Example 1, and details are not described herein.
Nano silicon nitride silicon materials manufactured in the present embodiment and embodiment 1 carry out same test material preparation, then test respectively
The compression strength of 1d, 3d, 7d, 28d, and the nano-silicon nitride cement base under corresponding number of days is tested with scanning electron microscope respectively
The microstructure of slurry.
Strength test results: 1d compression strength is 36.607Mpa；3d compression strength is 67.121Mpa；7d compression strength is
69.280MPa；28 days compression strength is 86.229MPa.
Microstructure analysis result: to the nano-silicon nitride cement base slurry under 1d, 3d, 7d, 28d in the present embodiment into
Row Micro-Structure Analysis, find slurry is presented fine and close structure, and air vent content is few.
Embodiment 3
Step 1 is replaced in the present embodiment are as follows: the nano-silicon nitride 0.192g after heat treatment is added, water-reducing agent additional amount
For 0.24g, it is 0.1% that water-reducing agent, which accounts for cement quality ratio, and it is 1000r/min that nano-silicon nitride, which carries out churned mechanically revolving speed, is stirred
Mixing the time is 3min, and the time for then carrying out ultrasonic disperse is 40min；Step 2 replacement are as follows: nano-silicon nitride suspension
72.432g, reference cement 240g, the ratio that nano-silicon nitride incorporation accounts for cement is 0.08%, other methods step and implementation
Example 1 is identical, and details are not described herein.
Nano silicon nitride silicon materials manufactured in the present embodiment and embodiment 1 carry out same test material preparation, then test respectively
The compression strength of 1d, 3d, 7d, 28d, and the nano-silicon nitride cement base under corresponding number of days is tested with scanning electron microscope respectively
The microstructure of slurry.
Strength test results: 1d compression strength is 37.109Mpa；3d compression strength is 58.734Mpa；7d compression strength is
65.502MPa；28 days compression strength is 86.645MPa.
Microstructure analysis result: to the nano-silicon nitride cement base slurry under 1d, 3d, 7d, 28d in the present embodiment into
Row Micro-Structure Analysis finds that compact structure, air bubble content are few.
Embodiment 4
Step 1 is changed to the nano-silicon nitride 0.48g after heat treatment is added in the present embodiment, water-reducing agent additional amount is
0.48g, it is 0.2% that water-reducing agent, which accounts for cement quality ratio, reference cement 240g, and nano-silicon nitride incorporation accounts for cement in the present embodiment
The ratio of sill is 0.2%, and other methods step is same as Example 1, and details are not described herein.
Material manufactured in the present embodiment and embodiment 1 carry out same test material preparation, then test respectively 1d, 3d, 7d,
The compression strength of 28d, and the micro- of nano-silicon nitride cement base slurry under corresponding number of days is tested with scanning electron microscope respectively
See structure.
Strength test results: 1d compression strength is 46.291Mpa；3d compression strength is 67.925Mpa；7d compression strength is
83.634MPa；28 days compression strength is 85.140MPa.
Microstructure analysis result: to the nano-silicon nitride cement base slurry under 1d, 3d, 7d, 28d in the present embodiment into
Row Micro-Structure Analysis finds that compact structure, air bubble content are few.
Reference examples 1
Reference examples 1 are the difference from embodiment 1 is that be omitted the nano-silicon nitride in the first step and second step, i.e. this control
Nano silicon nitride silicon materials are not mixed in cement-based material in example, weigh water 72g, water-reducing agent 0.096g, reference cement 240g, other
Method and step is same as Example 1, and details are not described herein.
The cement-based material for preparing in this reference examples and embodiment 1 carry out same test material preparation, then test respectively 1d,
The compression strength of 3d, 7d, 28d, and the nano-silicon nitride cement base tested under corresponding number of days respectively with scanning electron microscope is starched
The microstructure of body.
Strength test results: 1d compression strength is 33.251MPa；3d compression strength is 53.047MPa；7d compression strength is
64.807MPa；28d compression strength is 81.182MPa.
Microstructure analysis result: having the presence of micro-crack and stomata inside test block, dense structure's degree is not high.
Reference examples 2
Reference examples 2 are the difference from embodiment 1 is that the heating temperature of the heat treatment of nano-silicon nitride is 200 DEG C, when heating
Between be 30min, other methods step is same as Example 1, and details are not described herein.
The cement-based material for preparing in this reference examples and embodiment 1 carry out same test material preparation, then test respectively 1d,
The compression strength of 3d, 7d, 28d, and the nano-silicon nitride cement base tested under corresponding number of days respectively with scanning electron microscope is starched
The microstructure of body.
Strength test results: 1d compression strength is 34.927MPa；3d compression strength is 56.607MPa；7d compression strength is
65.393MPa；28d compression strength is 72.021MPa.
Microstructure analysis result: the test block surface in this reference examples has obvious bubble, and also contains among broken test block
There are a small amount of minute bubbles.
Reference examples 3
Reference examples 3 the difference from embodiment 1 is that nano-silicon nitride without heat treatment, be added without Overheating Treatment after
Nano-silicon nitride 0.120g, step 2 replacement are as follows: nano-silicon nitride suspension 72.600g, reference cement 240g, other methods
Step is same as Example 1, and details are not described herein, and the ratio that nano-silicon nitride incorporation accounts for cement-based material is 0.04%.
Nano silicon nitride silicon materials manufactured in the present embodiment and embodiment 1 carry out same test material preparation, then test respectively
The compression strength of 1d, 3d, 7d, 28d, and the nano-silicon nitride cement base under corresponding number of days is tested with scanning electron microscope respectively
The microstructure of slurry.
Strength test results: 1d compression strength is 36.758Mpa；3d compression strength is 56.706Mpa；7d compression strength is
72.788MPa；28 days compression strength is 77.599MPa.
Microstructure analysis result: the test block air bubble content in this reference examples is more, and has apparent crackle.
The flexural strength that the nano-silicon nitride cement base slurry prepared in above-described embodiment and reference examples carries out 28d is surveyed
Examination, and by reference examples 1,2,3 compression strength and flexural strength compare with the data in embodiment 1, obtained data
As a result as shown in Table 1 below.
The compression strength and flexural strength of cement base slurry in the different embodiments of table 1 and reference examples
It is known that embodiment 1 is compared with reference examples 1 from table, the cement base slurry 28 of nano-silicon nitride preparation is added
Its compression strength improves 24.60%, and 28 days flexural strengths improve 19.8%；Resistance to compression in embodiment 2 and in embodiment 3
Intensity and flexural strength equally also excellent data in reference examples 1, illustrate that being added to nano-silicon nitride significantly enhances cement
The compression strength and flexural strength of sill.
Reference examples 2 are compared with embodiment, and the heating temperature of the heat treatment for the nano-silicon nitride being added in reference examples 2 is 200
DEG C, compression strength and flexural strength numerical value illustrate nanometer also below compression strength and flexural strength in corresponding embodiment 1-4
Silicon nitride heat treatment temperature has larger impact to the performance of cement base slurry.
It is added compared to the nano-silicon nitride being added after being heat-treated, in reference examples 3 strong without the nano-silicon nitride of Overheating Treatment
Degree has apparent reduction, illustrates that the nano-silicon nitride without Overheating Treatment is added, the intensity of cement matrix slurry body can drop significantly
It is low.
All there is bubble in the cement base slurry test block surface prepared in reference examples 2-3, and reference examples 3 are without Overheating Treatment
The cement base slurry that is prepared into of nano-silicon nitride in have apparent crackle, nano-silicon nitride is after the heat treatment of suitable temperature
It can reduce air bubble content, be after XRD analysis, to find nano silicon nitride because nano silicon nitride silicon face contains impurity component
Silicon face contains ammonium chloride, and after Overheating Treatment, ammonium chloride can be removed, substantially reduce the air bubble content of slurry test block, disappeared
The defects of stomata caused by bubble removing, crackle, increase the compactness of microstructure, thus improve material compression strength and anti-folding
Intensity.
In summary: nano-silicon nitride of the invention enhances cement-based material, is added in cement-based grout preparation process
Nano-silicon nitride, nano-silicon nitride carry out heat treatment and decentralized processing, are then added in cement grout in certain proportion, and
The materials such as additive are added, to improve the physical and mechanical property (compression strength and flexural strength) of cement-based material and durable
Property；Nano-silicon nitride of the invention enhances cement-based material, and microstructure is even closer, porosity is reduced, to improve
The mechanical property of cement slurry greatly enhances；In 0.16% incorporation of nano-silicon nitride, 28d compression strength improves 24.6%,
The defects of 28 days flexural strengths improve 19.8%, and the compact structure of cement matrix slurry body, internal flawless.
The above description is only a preferred embodiment of the present invention, is not intended to restrict the invention, for those skilled in the art
For member, the invention may be variously modified and varied.All within the spirits and principles of the present invention, it is made it is any modification,
Equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of nano-silicon nitride enhancing cement-based material, which is characterized in that the preparation of the cement-based material
Method the following steps are included:
The heat treatment of S1, nano-silicon nitride
Nano-silicon nitride is contained up in heatproof container, baking oven is put into and is heated, makes the impurity of nano silicon nitride silicon face
It overflows, takes out nano-silicon nitride after heat treatment；
The decentralized processing of S2, nano-silicon nitride
Water is added into container, then the nano-silicon nitride after heat treatment is put into container, then dispersing agent is added into container,
After addition, the suspension of nano-silicon nitride is formed；Nano silicon nitride silicon suspension is subjected to mechanical stirring, mechanical stirring terminates
After carry out ultrasonic disperse；
The preparation of S3, cement-based material
By ultrasonic disperse in step S2, treated that nano silicon nitride silicon suspension is added into blender, then into blender plus
Enter water and cement, obtain cement-based material mixed liquor, cement-based material mixed liquor is stirred, obtains nano-silicon nitride enhancing
Cement-based material.
2. the preparation method of nano-silicon nitride enhancing cement-based material as described in claim 1, which is characterized in that in step S1
Heating temperature to nano-silicon nitride heat treatment is 325 DEG C~375 DEG C, and heating time is 30min~120min.
3. the preparation method of nano-silicon nitride enhancing cement-based material as described in claim 1, which is characterized in that in step S2
The dispersing agent is polycarboxylic acids dehydragent；
Preferably, the additional amount of the dispersing agent accounts for the 0.01%~0.5% of cement quality.
4. the preparation method of nano-silicon nitride enhancing cement-based material as described in claim 1, which is characterized in that in step S3
The additional amount of nano silicon nitride silicon suspension is no more than the 2% of nano-silicon nitride enhancing cement-based material；
Preferably, the additional amount of nano silicon nitride silicon suspension accounts for the 0.01% of nano-silicon nitride enhancing cement-based material in step S3
~0.2%.
5. the preparation method of nano-silicon nitride enhancing cement-based material as described in claim 1, which is characterized in that in step S2
Nano silicon nitride silicon suspension is subjected to the churned mechanically time as 2min~7min, the time of ultrasonic disperse is no less than 30min.
6. the preparation method of nano-silicon nitride enhancing cement-based material as claimed in claim 5, which is characterized in that the nanometer
It is 500r/min~1000r/min that silicon nitride suspending liquid, which carries out churned mechanically revolving speed,.
7. the preparation method of nano-silicon nitride enhancing cement-based material as described in claim 1, which is characterized in that in step S3
The ratio of mud that water and cement into the blender is added is 0.28~0.40.
8. the preparation method of nano-silicon nitride enhancing cement-based material as described in claim 1, which is characterized in that in step S3
It is first to mix slowly 120s to the agitating mode that cement-based material mixed liquor is stirred, revolving speed is 135r/min~145r/
Then min stops stirring 15s, then quickly stirring 120s, revolving speed are 275r/min~295r/min, then stops.
9. the preparation method of nano-silicon nitride enhancing cement-based material as described in claim 1, which is characterized in that in step S1
The average particle size of nano-silicon nitride is 10nm~30nm.
10. a kind of preparation method preparation of the nano-silicon nitride enhancing cement-based material as described in claim 1~9 is any is received
Rice silicon nitride enhances cement-based material.
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| CN115636647B (en) * | 2022-11-20 | 2023-09-29 | 中电建路桥集团有限公司 | Concrete based on micro-nano components and preparation method thereof |
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