CN103992114A - Preparation method of boron carbide ceramic powder dispersion - Google Patents
Preparation method of boron carbide ceramic powder dispersion Download PDFInfo
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- CN103992114A CN103992114A CN201410218514.4A CN201410218514A CN103992114A CN 103992114 A CN103992114 A CN 103992114A CN 201410218514 A CN201410218514 A CN 201410218514A CN 103992114 A CN103992114 A CN 103992114A
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Abstract
The invention discloses a preparation method of a boron carbide ceramic powder dispersion, which comprises the following steps: adding 0.01-10 wt% of polyethyleneimine and 0.01-10 wt% of polyethyleneglycol into water, uniformly mixing, adding 10-50 wt% of boron carbide ceramic powder, and uniformly mixing; adding the mixture into a ball mill, and carrying out ball milling for more than 3 hours to obtain a suspension; and standing the suspension for 15-60 minutes to remove the deposited boron carbide ceramic powder particles, thereby obtaining the boron carbide ceramic powder dispersion. The method can be used for obtaining the simple cheap environment-friendly boron carbide ceramic powder dispersion and providing a slurry for preparing a ceramic system by slip casting, gel cast forming, injection forming and other wet forming processes.
Description
Technical field
The present invention relates to powder dispersion technology field, particularly a kind of preparation method of boron carbide ceramics powder dispersion.
Background technology
Boron carbide ceramics is a kind of important engineering materials.Its hardness is only second to diamond and cubic boron nitride, and under high temperature, its constant hot hardness (> 30GPa) will be better than diamond and cubic boron nitride from far away.Its theoretical density is 2.52g/cm
3, fusing point is 2450 ℃, microhardness is 4950kgf/mm
2.Boron carbide ceramics has that quality is light, semi-conductor physical property, absorb seed, mill efficiency high, with the feature such as the equal Fails To Respond of strong acid and strong base.Owing to having the performance of above-mentioned excellence, boron carbide ceramics is widely used in the fields such as metallurgy, chemical industry, machinery, aerospace.For example: norbide can be used as abrasive machining jewel, pottery, bearing and cutter; Can be in field of metallurgy as refractory materials; The norbide of densification can also be made into nozzle, mechanical sealing member or bullet resistant material etc.; Norbide also can absorb because having larger thermal capture interface the protection that a large amount of seeds is used to nuclear reactor.
Ultrafine powder, because particle is tiny and have very large surface energy, disperses very easily spontaneous reunion to form secondary powder particle to reduce the total surface energy of system in liquid.Under the condition of powder suspension infiltration, if there is coacervate in powder, easily cause material regional area to occur component segregation, the structure of material and performance are had to many bad impacts.Therefore, the agglomeration of powder and how to take effective method to reduce even and eliminate and reunite, is in the preparation of powder and the problem that should pay close attention in using to reach powder good dispersion this purpose in suspension.
The dispersion state of powder in liquid phase medium, is mainly subject to interactional impact the between powder particle.At present, make powder particle equably stable dispersion in liquid phase medium, conventionally have following three kinds of stable mechanisms:
(1) electrostatic stabilization mechanism (electrostatic double layer stable mechanism): in liquid phase medium, by regulating pH value or adding suitable ionogen, make powder particle surface attract electrically contrary ion to form electrostatic double layer, coulombic repulsion between electrostatic double layer greatly reduces the gravitation that powder particle is reunited, thereby powder particle is disperseed.The surface potential of powder particle and strength of solution are two topmost factors of powder particle electrostatic stabilization in liquid phase medium.
(2) sterically hindered stable mechanism: add electroneutral high molecular polymer in liquid phase medium, powder particle surface adsorbed polymer polymkeric substance, has formed a powder particle micelle being wrapped by.Sterically hindered effect mutual between high molecular polymer produces repulsive force, makes effect suspension stabilization.Powder particle disperses in the organic solvent of low-k (being low-pole or nonpolar), is usually considered to be undertaken by sterically hindered mechanism.As added polyoxyethylene glycol, peg molecule to produce sterically hindered effect in liquid phase reaction, thereby hinder powder particle, further reunite and grow up.
(3) electric sterically hindered mechanism: selecting a polymer dielectric that not only provided sterically hindered effect simultaneously but also had an electrostatic repulsion is dispersion agent, regulate the pH of suspension, make the polymer dielectric of particle surface absorption reach capacity adsorptive capacity and maximum degree of ionization, thereby increase double electrode layer repulsion, makes the uniform and stable dispersion of powder particle.Conventional dispersion agent is high molecular polymer ionogen, anionic polymer electrolyte, and ammonium salt or the sodium salt of polyacrylic acid and polymethyl acrylic acid of take is representative.
The dispersion means of powder particle in liquid, can be divided into three major types substantially:
(1) select respective media: by selecting suitable dispersion medium can obtain dispersion suspension comparatively fully, this is that character by powder self decides.For the liquid medium disperseing, be divided into polarizable medium and nonpolar medium two classes.Select the principle of dispersion medium to be: polarity powder particle is easy to disperse in polarizable medium, and nonpolar powder particle is easy to disperse in nonpolar medium.
(2) add dispersion agent: by adding dispersion agent can provide the good distribution of polarity powder particle in polarizable medium needed physical and chemical condition.The interpolation of dispersion agent can increase the mutually exclusive effect between powder particle.Conventional dispersion agent mainly contains two kinds: inorganic electrolyte, and as sodium polyphosphate, water glass, sodium hydroxide etc., organic high molecular polymer, as tensio-active agents such as polypropylene phthalein amine series, tannin.The dissemination of tensio-active agent is mainly manifested in it to the adjustment of particle surface wettability, because it has good dissemination, in industry, is widely used.
(3) mechanical force is disperseed: the dispersion under mechanical force is considered to simple physical dispersion conventionally, is mainly a kind of form that nanoparticle is fully disperseed in medium by mechanical energy such as extraneous shearing force or impact forces.By dispersion system being applied to physics, the chemical property that mechanical force can cause material in system and following series of chemical to reach dispersion object.The destruction that powder particle is reunited is mainly by mechanical size degradation and power ultrasonic size degradation.The mechanical size degradation of coacervate is mainly by impacting, and the mechanical forces such as shearing and stretching realize, and are that a kind of simple and easy to do means specific form has: grinding distribution, colloidal mill dispersion, Ball milling, sand milling dispersion, high-speed stirring etc.Ultrasonic dispersion is needing suspension to be processed to be directly placed in ultrasonic field, controlling suitable ultrasonic frequency and action time, so that particle fully disperses.On the one hand, ultrasonic wave form with standing wave in granular system is propagated, and makes particle be subject to periodically stretching and compression; On the other hand, ultrasonic wave can produce " cavitation " effect in liquid, and particle is disperseed.
In EP1153652, recorded a kind of by the mixed powder of wolfram varbide and cobalt (hard metal powders mixture) part added other mechanically resistant materials as the condition of TiC, TaC, TiN under, be scattered in the method for the medium of the moisture or ethanol that has added cationic polyelectrolyte polymine.Here, by interpolation massfraction 0.1 to 10%, preferred mass mark, be 0.1-1%, molar mass is 5000-50000, preferably 10000 to 30000g/mol polymine (PEI) is realized the good dispersion of hard metal powders mixture in water.
In WO93/21127, prepared the nano ceramic powder of surface modification as Si
3n
4, SiC, Al
2o
3deng, approach, be to utilize low molecular organic compound (molar mass is up to 500g.mol) that each unmodified powder is scattered in to water or organic solvent as in alcohols.
In DE19751355, having recorded a kind of method that fine particulate inorganic powder is distributed to water preferably or water-bearing media, is wherein the material of biogenetic derivation as the material disperseing, as sugared derivative, starch derivative or chitin derivatives.Here refer to especially and in water-bearing media, produce long stable dispersions.
The shortcoming of the method realizing according to prior art is: it is dispersed in powder in the medium of organic solvent medium or organic solvent-water medium rather than pure water, and cost is high and unfriendly to environment.The powder of its dispersion has comprised that cemented carbide powder, ceramic powder are partly if the nanometer powder of TiC, TaC, TiN and part is as nanometer Si
3n
4, SiC, Al
2o
3deng.But for specific boron carbide ceramics powder dispersion preparation, without corresponding research, invent at present.
Summary of the invention
The preparation method who the object of this invention is to provide a kind of boron carbide ceramics powder dispersion, solves the problem that there is no the corresponding preparation method of boron carbide ceramics powder dispersion in prior art.
For addressing the above problem, the present invention by the following technical solutions:
A preparation method for boron carbide ceramics powder dispersion, comprises the following steps:
By mass percentage, 0.01～10% polymine and 0.01～10% polyoxyethylene glycol are added to the water, mix, then add 10～50% boron carbide ceramics powder, mix; Join afterwards ball milling 3h in ball mill and obtain above suspension; The boron carbide ceramics powder particle of the standing 15～60min of suspension being removed to coagulation, obtains boron carbide ceramics powder dispersion.
Described boron carbide ceramics powder quality per-cent is 30～40%, and described polymine mass percent is 1～3%, and described polyoxyethylene glycol mass percent is 3～5%.
Described polymine mass percent is 2.5%.
Described boron carbide ceramics diameier is 1～40um.
The molecular weight of described polyoxyethylene glycol is 5000～20000.
Described Ball-milling Time is 3～4h.
Beneficial effect of the present invention: by the present invention, can obtain the boron carbide ceramics powder dispersion on cheap and simple and environmentally friendly ground, be provided for the wet-formed legal systems such as casting, gel pouring shaping, injection forming for the slurry of ceramic systems.
Accompanying drawing explanation
Fig. 1 is the SEM figure of the boron carbide ceramics powder that adopts of embodiment.
Fig. 2 is that the dispersing property of the corresponding dispersion of the different Ball-milling Times of embodiment 1 characterizes.
Fig. 3 is that the dispersing property of the corresponding dispersion of embodiment 2 different dispersion characterizes.
Fig. 4 is that the dispersing property of the corresponding dispersion of embodiment 3 different sorts dispersion agents characterizes.
Fig. 5 is that the dispersing property of the corresponding dispersion of embodiment 4 different mass mark polymines characterizes.
Embodiment
Below in conjunction with embodiment, the present invention is done further and explained.The following example is only for the present invention is described, but is not used for limiting practical range of the present invention.
A kind of preparation method of boron carbide ceramics powder dispersion, take water as dispersion medium, water miscible polymine (PEI) and polyoxyethylene glycol (PEG) be dispersion agent, comprise the following steps: by mass percentage, 0.01～10% polymine and 0.01～10% polyoxyethylene glycol are added to the water, mix, add again 10～50% boron carbide ceramics powder, mix; Join afterwards in ball mill ball milling 3h above preferably 3～4h obtain suspension; The boron carbide ceramics powder particle of the standing 15～60min of suspension being removed to coagulation, obtains boron carbide ceramics powder dispersion.
The boron carbide ceramics powder density that embodiment adopts is about 2.6g/cm
3, the boron carbide ceramics powder that takes a morsel arbitrarily, is evenly placed on scanning electronic microscope experiment table, observes its size distribution, and as shown in Figure 1, the particle diameter of boron carbide ceramics powder is at 1～40um.Boron carbide ceramics powder shared mass percent in suspension is 10～50%, preferably 30～40%.
Polymine is generally water miscible colourless or faint yellow glutinous thick liquid, commercially available product is generally the aqueous solution of 10%～50% concentration, as Sigma-Aldrich company is numbered 50% aqueous products of 482595 molecular-weight average 1300 and is numbered 03880 molecular weight can be for the present invention at 50% aqueous products of 600000～1000000 scopes etc.Polymine shared mass percent in suspension is 0.01%～10%, is preferably 1～3%, more preferably 2.5%.
Polyoxyethylene glycol is the hard wax-like thin slice solid of white, and molecular weight is 5000～20000.Polyoxyethylene glycol shared mass percent in suspension is 0.01～10%, is preferably 3～5%.
For characterizing boron carbide ceramics powder particle, in the stability of suspension and the method for dispersibility, be: observe suspension and clarify/be suspended the time dependent changing conditions in interface.Embodiments mode is suspension is poured in test tube and demarcate liquid level elemental height h
0, at interval of phase same amount of time, measure suspension and clarify/be suspended the height h at interface
i(i=1,2,3,4 ...), for example within every and a half hours, measure an interfacial level, after several hours, according to interfacial level, just judge the stability of suspension and draw the time dependent curve of interfacial level.The liquid level of suspension clarification part reduces sooner, and suspension stability and the dispersibility of ceramic particle are poorer.
Embodiment 1
Under the prerequisite that the present embodiment remains unchanged at other preparation condition, change Ball-milling Time, observe different Ball-milling Times for the impact of dispersion stability.
1.75g polymine (mass percent is 2.2%), 2.5g polyoxyethylene glycol (mass percent is 3.15%) are dissolved in 50ml deionized water, mix, and then stir and add 25g boron carbide ceramics powder (mass percent is 31.5%); Ball milling certain hour (being respectively 0h, 1h, 3h, 5h) in planetary ball mill respectively afterwards; Standing 30min removes the boron carbide ceramics powder particle of coagulation, obtains boron carbide ceramics powder dispersion.
The dispersed characterization result of the corresponding dispersion of different Ball-milling Times as shown in Figure 2.The demonstration of dispersing property characterization result, Ball milling method can improve the dispersiveness of suspension significantly.Along with the increase of Ball-milling Time, the dispersing property of suspension improves lifting gradually, when Ball-milling Time surpasses 3h, just can obtain above dispersed suspension preferably.Although for the mixed powder of ball milling, Ball-milling Time is longer merely, obtains suspension dispersing property also just better.But for the whole preparation process of matrix material, the consideration needing for time cost and preparation, when Ball-milling Time is can make suspension comparatively stable within for some time between 3～4h for subsequent preparation process, although and long Ball-milling Time is beneficial to the dispersiveness that improves suspension, it there is no large profit to whole preparation process.
Embodiment 2
Under the prerequisite that the present embodiment remains unchanged at other preparation condition, select deionized water and dehydrated alcohol respectively as dispersion medium, observe different dispersion for the impact of dispersion stability.
1.75g polymine (mass percent is 2.2%), 2.5g polyoxyethylene glycol (mass percent is 3.15%) are dissolved in 50ml dispersion medium (being respectively deionized water, dehydrated alcohol), mix, and then stir and add 25g boron carbide ceramics powder (mass percent is 31.5%); Ball milling 3h in planetary ball mill afterwards; Standing 30min removes the boron carbide ceramics powder particle of coagulation, obtains boron carbide ceramics powder dispersion.
The dispersed characterization result of the corresponding dispersion of different media as shown in Figure 3.The demonstration of dispersing property characterization result, deionized water and dehydrated alcohol all play certain dissemination as dispersion medium to boron carbide ceramics powder.In the situation that other condition is certain, the dispersiveness of dehydrated alcohol boron carbide ceramics powder during as dispersion agent is poor, and about 2.5 hours, basic precipitation is completely.And when deionized water is during as dispersion agent, boron carbide powder has good dispersiveness, after 3 hours, still can keep certain interfacial level.Therefore, deionized water is comparatively suitable dispersion agent.
Embodiment 3
Under the prerequisite that the present embodiment remains unchanged at other preparation condition, select polymine, polyoxyethylene glycol, polymine+polyoxyethylene glycol respectively as dispersion agent, observe different dispersion agents for the impact of dispersion stability.
Dispersion agent (being respectively mass percent 3% polymine, mass percent 3% polyoxyethylene glycol, mass percent 1.2% polymine+mass percent 1.8% polyoxyethylene glycol) is dissolved in 50ml deionized water, mix, and then stir and add 25g boron carbide ceramics powder; Ball milling 3h in planetary ball mill afterwards; Standing 30min removes the boron carbide ceramics powder particle of coagulation, obtains boron carbide ceramics powder dispersion.
The dispersed characterization result of the corresponding dispersion of different sorts dispersion agent as shown in Figure 4.Dispersing property characterization result shows, uses separately polyoxyethylene glycol comparatively undesirable as dispersion agent result of use, and coagulation phenomenon occurs at short notice, cannot meet the demand in actual fabrication process; Polyoxyethylene glycol+polymine compound use is had to more good dispersing property as dispersion agent, suspension still can keep certain dispersiveness within standing 3h, although it also occurs the dispersed trend reducing later at about 3.5h, it can meet the requirement of actual fabrication process to stability of suspension; And use separately polymine effect to occupy between the two.Select from the above results polyoxyethylene glycol+polymine as composite dispersing agent.
Embodiment 4
Under the prerequisite that the present embodiment remains unchanged at other preparation condition, select the different polymine of massfraction, observe the polymine of different mass mark for the impact of dispersion stability.
By the polymine of certain mass percent (mass percent is respectively 1%, 2.5%, 3.5%), mass percent, be that 3.1% polyoxyethylene glycol is dissolved in 50ml deionized water, mix, and then stir and add 25g boron carbide ceramics powder; Ball milling 3h in planetary ball mill afterwards; Standing 30min removes the boron carbide ceramics powder particle of coagulation, obtains boron carbide ceramics powder dispersion.The dispersed characterization result of the corresponding dispersion of polymine of different mass mark as shown in Figure 5.Numbering 1,2,3 represents respectively polymine massfraction 1%, 2.5%, 3.5%.From result, when polymine massfraction is 2.5%, suspension has best dispersing property, dispersing property weakened at different degrees while being greater than or less than this proportioning.
Embodiment 5
By mass percentage, 0.01% polymine, 0.01% polyoxyethylene glycol are dissolved in deionized water, mix, and then stir the boron carbide ceramics powder that adds 10%; Afterwards at planetary ball mill ball milling 3h; Standing 15min removes the boron carbide ceramics powder particle of coagulation, obtains boron carbide ceramics powder dispersion.
The characterization result of dispersion stability prepared by the present embodiment is as shown in table 1:
Table 1
Embodiment 6
By mass percentage, 10% polymine, 10% polyoxyethylene glycol are dissolved in deionized water, mix, and then stir the boron carbide ceramics powder that adds 50%; Afterwards at planetary ball mill ball milling 4h; Standing 60min removes the boron carbide ceramics powder particle of coagulation, obtains boron carbide ceramics powder dispersion.
The characterization result of dispersion stability prepared by the present embodiment is as shown in table 2:
Table 2
Embodiment 7
By mass percentage, 0.01% polymine, 10% polyoxyethylene glycol are dissolved in deionized water, mix, and then stir the boron carbide ceramics powder that adds 10%; Afterwards at planetary ball mill ball milling 3h; Standing 15min removes the boron carbide ceramics powder particle of coagulation, obtains boron carbide ceramics powder dispersion.
The characterization result of dispersion stability prepared by the present embodiment is as shown in table 3:
Table 3
Embodiment 8
By mass percentage, 10% polymine, 0.01% polyoxyethylene glycol are dissolved in deionized water, mix, and then stir the boron carbide ceramics powder that adds 50%; Afterwards at planetary ball mill ball milling 4h; Standing 60min removes the boron carbide ceramics powder particle of coagulation, obtains boron carbide ceramics powder dispersion.
The characterization result of dispersion stability prepared by the present embodiment is as shown in table 4:
Table 4
Embodiment 9
By mass percentage, 1% polymine, 3% polyoxyethylene glycol are dissolved in deionized water, mix, and then stir the boron carbide ceramics powder that adds 30%; Afterwards at planetary ball mill ball milling 3h; Standing 30min removes the boron carbide ceramics powder particle of coagulation, obtains boron carbide ceramics powder dispersion.
The characterization result of dispersion stability prepared by the present embodiment is as shown in table 5:
Table 5
Embodiment 10
By mass percentage, 3% polymine, 5% polyoxyethylene glycol are dissolved in deionized water, mix, and then stir the boron carbide ceramics powder that adds 40%; Afterwards at planetary ball mill ball milling 4h; Standing 30min removes the boron carbide ceramics powder particle of coagulation, obtains boron carbide ceramics powder dispersion.
The characterization result of dispersion stability prepared by the present embodiment is as shown in table 6:
Table 6
Claims (6)
1. a preparation method for boron carbide ceramics powder dispersion, is characterized in that, comprises the following steps:
By mass percentage, 0.01～10% polymine and 0.01～10% polyoxyethylene glycol are added to the water, mix, then add 10～50% boron carbide ceramics powder, mix; Join afterwards ball milling 3h in ball mill and obtain above suspension; The boron carbide ceramics powder particle of the standing 15～60min of suspension being removed to coagulation, obtains boron carbide ceramics powder dispersion.
2. the preparation method of boron carbide ceramics powder dispersion according to claim 1, it is characterized in that, described boron carbide ceramics powder quality per-cent is 30～40%, and described polymine mass percent is 1～3%, and described polyoxyethylene glycol mass percent is 3～5%.
3. the preparation method of boron carbide ceramics powder dispersion according to claim 2, is characterized in that, described polymine mass percent is 2.5%.
4. the preparation method of boron carbide ceramics powder dispersion according to claim 1, is characterized in that, described boron carbide ceramics diameier is 1～40um.
5. the preparation method of boron carbide ceramics powder dispersion according to claim 1, is characterized in that, the molecular weight of described polyoxyethylene glycol is 5000～20000.
6. the preparation method of boron carbide ceramics powder dispersion according to claim 1, is characterized in that, described Ball-milling Time is 3～4h.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105198479A (en) * | 2015-10-12 | 2015-12-30 | 北京东泰富博新材料科技股份有限公司 | Method for preparing starch-containing ceramic slurry from diatomite |
| CN105967690B (en) * | 2016-04-22 | 2018-08-03 | 合肥工业大学 | A kind of method of superfine powder and large-size particles batch mixing |
| CN109678528A (en) * | 2019-01-23 | 2019-04-26 | 佛山市山有海科技有限公司 | A kind of ceramics degumming agent and its preparation method and application |
| CN109721382A (en) * | 2018-12-29 | 2019-05-07 | 中国科学院长春光学精密机械与物理研究所 | A kind of ceramic particle suspended nitride and its preparation method and application |
| CN112174210A (en) * | 2020-09-23 | 2021-01-05 | 烟台佳隆纳米产业有限公司 | Preparation method of aqueous dispersion-free nano cesium tungsten oxide coating |
| CN112608717A (en) * | 2020-12-17 | 2021-04-06 | 长沙蓝思新材料有限公司 | Coarse grinding fluid and preparation method thereof |
| CN114656277A (en) * | 2022-03-17 | 2022-06-24 | 南通三责精密陶瓷有限公司 | Method for manufacturing environment-friendly pressureless sintering boron carbide ceramic material |
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2014
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105198479A (en) * | 2015-10-12 | 2015-12-30 | 北京东泰富博新材料科技股份有限公司 | Method for preparing starch-containing ceramic slurry from diatomite |
| CN105198479B (en) * | 2015-10-12 | 2016-05-11 | 北京东泰富博新材料科技股份有限公司 | A kind of method of utilizing diatomite to prepare starch-containing ceramic size |
| CN105967690B (en) * | 2016-04-22 | 2018-08-03 | 合肥工业大学 | A kind of method of superfine powder and large-size particles batch mixing |
| CN109721382A (en) * | 2018-12-29 | 2019-05-07 | 中国科学院长春光学精密机械与物理研究所 | A kind of ceramic particle suspended nitride and its preparation method and application |
| CN109678528A (en) * | 2019-01-23 | 2019-04-26 | 佛山市山有海科技有限公司 | A kind of ceramics degumming agent and its preparation method and application |
| CN112174210A (en) * | 2020-09-23 | 2021-01-05 | 烟台佳隆纳米产业有限公司 | Preparation method of aqueous dispersion-free nano cesium tungsten oxide coating |
| CN112608717A (en) * | 2020-12-17 | 2021-04-06 | 长沙蓝思新材料有限公司 | Coarse grinding fluid and preparation method thereof |
| CN114656277A (en) * | 2022-03-17 | 2022-06-24 | 南通三责精密陶瓷有限公司 | Method for manufacturing environment-friendly pressureless sintering boron carbide ceramic material |
| CN114656277B (en) * | 2022-03-17 | 2022-12-27 | 南通三责精密陶瓷有限公司 | Method for manufacturing environment-friendly pressureless sintering boron carbide ceramic material |
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Application publication date: 20140820 |