CN103979938A - Deep-sea pressure resistant alumina ceramic hollow floating ball and preparation method thereof - Google Patents
Deep-sea pressure resistant alumina ceramic hollow floating ball and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a deep-sea pressure resistant alumina ceramic hollow floating ball and a preparation method thereof. The preparation method comprises the following steps: 1,preparing reaction raw materials: uniformly ball-milling and mixing alumina powder with auxiliary agents for sintering, and dissolving acrylamide and a crosslinking agent N,N-methylene-bisacrylamide with stirring to obtain a premix solution; 2, rotating gel casting: mixing the ceramic powder with the premix solution with stirring, adding auxiliary agents, injecting the mixture into a spherical mold cavity after vacuum-degassing, rotating a mold, solidifying and shaping the mixture, and obtaining an alumina floating ball green body after drying; 3, binder removal and sintering: heating the dried alumina floating ball green body at a temperature of 300-800 DEG C to carry out binder removal, and carrying out sintering at a temperature of 1600-1800 DEG C to obtain a sintered body; 4, glazing: immersing the sintered body in glaze slip and carrying out glazing at a temperature of 500-800 DEG C. The floating ball has the following characteristics: the weight percentage of alumina is 94-99.9%, the outer diameter is 40-300 mm, the thickness of the spherical shell is 2-12 mm, the thickness deviation of the spherical shell is 0.1-2.5 mm, and the hydrostatic pressure the floating ball can resist is 150 MPa. The invention can be applied in deep sea of 11000 meters deep.
Description
Technical field
The present invention relates to a kind of ball float and preparation method thereof, be specifically related to withstand voltage alumina-ceramic hollow float in a kind of deep-sea and preparation method thereof.
Background technology
The area of the earth 71% is covered by ocean, and being greater than mesopelagic, the region, deep-sea of 200 meters, the degree of depth accounts for 91% of whole ocean area, the wide deep-sea depth of water can reach myriametre, pressure is large, and water temperature is low, there is no illumination, throughout the year in dark state, anoxic, food is rare, so be once considered to waste rough ground and life forbidden zone.Harsh environment marches deep-sea to the mankind and has proposed challenge, until last century, the eighties developed country just had the ability to explore deep-sea, so deep-sea is last piece virgin land of the earth, the focus of Ye Shi new millennium various countries " blueness is enclosed the land " motion sharp fight.
Deep-sea battle is resource battle after all.According to statistics, world's deep-sea oil gas proven reserve have accounted for the more than 65% of marine oil and gas proven reserve at present; The total amount of gas hydrate in ocean is (1 ~ 5) * 10
15cubic meter; Polymetallic nodule approximately have 5,000 hundred million tons in ocean, are mainly enriched in 4000 ~ 6000 meters of degree of depth; Cobalt-bearing crust content in ocean can reach 1,000,000,000 tons, is mainly distributed in 500 ~ 4000 meters of degree of depth; Places up to a hundred submarine hydrothermal solution Polymetal Sulphide Ores content reaches 600,000,000 tons, is distributed in 1500 ~ 4000 meters of degree of depth; Thousands of kinds of true tumors have been found at deep-sea, and most species are that deep-marine-environment is exclusive.Therefore, necessary, the abundant energy of world's future development and strategic resource are being contained in deep-sea.The external interdependency of China's oil in 2011, up to 56.5%, surpasses barrier line 50%, and the risk of having aggravated national energy security is accelerated deep-sea oil gas exploitation imperative.1212 meters of China's South Sea mean depths, petroleum resources are between 230 ~ 30,000,000,000 tons, and Sweet natural gas total amount is about 16 tcms, accounts for 1/3rd of Chinese Petroliferous total resources, and 70% hydrocarbon resources is in pelagic realm.Therefore the deep-sea detecting equipment preparation that " flood dragon " number be representative of, take has great strategic significance.
At present, bathyscaph mainly comprises manned underwater vehicle and unmanned underwater vehicle, and wherein unmanned underwater vehicle includes cable remote-operated vehicle (ROV) and without autonomous underwater vehicle (AUV) two kinds of cable.The maximum diving depth of most manned deep-sea vehicles is 7000 meters of left and right, and " deep-sea challenger " number bathyscaph that Jin You U.S. director James Ka Meilong participates in making can dive to the 11000 meter degree of depth.In addition, existing many advanced unmanned underwater vehicles can the extremely same degree of depth of dive.For these bathyscaphs, one of most important versatility material is the solid buoyancy material of using as buoyancy compensation.During the actual use of buoyancy material, need long period of soaking in water, require its water-fast, withstand voltage, corrosion-resistant and shock resistance.Especially every increase 100m degree of depth in ocean, the pressure that object is subject to just will increase approximately 10 normal atmosphere, i.e. 1MPa.Dive to the 11000 meter degree of depth needs to bear the pressure of 110MPa so.Therefore, the buoyancy material using in deep-sea requires both to have high intensity very low density again, but also should have water-fast, corrosion-resistant and shock proof characteristic.Requirement of strength for the solid buoyancy material using at different depths is different, and the depth of water increases, the corresponding increase of intensity of buoyancy material, and density increases thereupon, but buoyancy factor reduces.In addition, the upper high strength buoyancy material using of deep-sea equipment also should have water-intake rate low, inhale the features such as the isorrheic time is short.
The 7000m manned underwater vehicle solid buoyancy material of U.S. Emerson & Cuming company development, density is 0.561g/cm
3, can be used for the 7000m depth of water.This material is to be evenly distributed on by the micron-sized hollow glass micropearl of diameter a kind of matrix material solidifying to form in resin, and wherein hollow glass micropearl accounts for 60% ~ 70% volume, therefore has lower density.But if dive is when darker, buoyancy material need to improve intensity to sacrifice autologous density.For equal buoyancy is provided, bathyscaph needs to assemble more buoyancy material, causes bulkyly, and dynamic performance declines." deep-sea challenger " number manned deep-sea vehicle is by add fiber on the basis of solid buoyancy material, and further the mechanical property of strongthener solves this problem, and its ultimate compression strength can reach 152MPa, and density is only also 0.69 g/cm
3.In addition, the large unmanned bathyscaph of the degree of depth is except using this type of buoyancy material, also use a kind of hollow ceramic ball as buoyancy material, this Ceramic Balls diameter is about 90mm, and shell thickness is only 1.6mm, and weight is about 140g, because pottery has high specific strength and low density, so this buoyant spheres can provide larger buoyancy, increase the payload capability of bathyscaph, be a kind of excellent combination property buoyancy material.But at present very few about the open experimental data of this deep-sea large-size ceramic buoyant spheres, its preparing craft is also in confidential state.Therefore its application still relies on external import, has restricted the development of the deep-sea unmanned bathyscaph of China.Therefore, the development of this large-size ceramic buoyant spheres is all significant in science mechanism and engineering Application Areas.
About this ceramic buoyant spheres, there are two kinds of preparation methods at present.Chinese patent ZL 200710144489.X is used stupalith first to make scarce hole spherical shell and port lid two portions of hollow ball, then by lacking hole spherical shell and port lid shrink-fit, forms a complete hollow ball base, finally by double sintering, forms ceramic hollow ball float.But the difficulty that this method preparation lacks hole spherical shell is larger, and the shrink-fit tooling cost of spherical shell and port lid is higher, in double sintering process, can the bonding that realize scarce hole spherical shell and port lid also need to be investigated, and is not therefore effective preparation method.Chinese patent 93118293.X propose to be used that to take aluminum oxide and silicon oxide be material, prepares the ceramic hollow ball of diameter 2-10cm by the mode of rotation injection forming.But green density and intensity are lower during due to rotation injection forming, and due to density of material difference, spherical shell is inner can produce component gradient, and then in sintering process, produces internal stress, causes strength degradation.In addition, the hollow ball profile of acquisition only can guarantee it is roughly ball-type, and low its anti-pressure ability that causes of sphericity declines, and therefore this hollow ball can not be used as deep-sea pressure-resistant floating ball.
Summary of the invention
The object of the invention is to, withstand voltage alumina-ceramic hollow float in a kind of deep-sea and preparation method thereof is provided, to overcome the existing above-mentioned shortcoming and defect of prior art.
Gelcasting Technique is a kind of new shaping mechanism that traditional slip-casting shaping process combines with polymerization theory.Its ultimate principle is in high solid phase, low viscous ceramic slurry, mixes the organic monomer of lower concentration.After adding initiator cast, there is home position polymerization reaction under certain condition in the organic monomer in slip, common in conjunction with forming firm tridimensional network with ceramic particle, by most of water seal in network and make slip immediately original position solidify, thereby make ceramic body custom-molded in place.Then carry out the demoulding, be dried, remove organism, sintering, can obtain required ceramic part.Even green body, density that this forming method obtains are high, intensity is large, can realize brilliant dead size moulding, are applicable to having thinner base substrate rapid shaping.And can carry out mechanical workout after body drying, reduce post-production cost.Therefore, by gel casting process, combining to prepare large-size ceramic hollow float with rotoforming is a kind of effective way.
The technical problem that will solve required for the present invention, can be achieved through the following technical solutions:
As a first aspect of the present invention, a kind of deep-sea is withstand voltage alumina-ceramic hollow float, is characterized in that, according to mass percent meter, its formula is:
Aluminum oxide 94% ~ 99.9% wt;
Sintering aid 0.1% ~ 6% wt.
By alumina-ceramic, be made, wherein the massfraction of aluminum oxide is 94% ~ 99.9% wt, and all the other compositions are comprised of sintering aid.
Further, described sintering aid is any one or combination of magnesium oxide, silicon oxide, and its total content is 0.1% ~ 6%wt.
Further, described alumina-ceramic hollow float external diameter is distributed in 40 ~ 300mm, and the shell thickness of described alumina-ceramic hollow float is 2 ~ 12mm, and the shell thickness deviation of described alumina-ceramic hollow float is 0.1 ~ 2.5mm.
Further, the maximum opposing of described hollow float hydrostaticpressure is 150MPa.
As a second aspect of the present invention, the preparation method of a kind of deep-sea is withstand voltage alumina-ceramic hollow float, is characterized in that, comprises the following steps:
Step 1, ready reaction raw material: aluminum oxide is mixed with sintering aid ball milling, acrylamide and linking agent N,N methylene bis acrylamide are dissolved in to the abundant acquisition premixed liquid that stirs in deionized water;
Step 2, rotation gel injection: by ceramic powder and premixed liquid mix and blend, add dispersion agent, catalyzer, initiator, after vacuum outgas, inject spherical cavity, by all-directional rotation, slurry is evenly attached on ball cavity wall, then control temperature and realize curing molding, after being dried, obtain aluminum oxide ball float green compact;
Step 3, come unstuck and sintering: by dry ceramic ball float base substrate 300 ~ 800
obetween C, heating is come unstuck, 1600 ~ 1800
obetween C, carry out sintering, obtain fine and close sintered compact;
Step 4, glazing: sintered compact is flooded in glaze slip, and 500 ~ 800
obetween C, heat, at its surface coverage layer of transparent ceramic glaze layer.
In step 2, described alumina-ceramic hollow float, by rotation gel injection technological forming, comprises the following steps:
A1) aluminum oxide and sintering aid are added in ball grinder, then add the alumina-ceramic abrading-ball that doubles its quality, by both ball millings in spirituous solution, it is evenly mixed, then dry, sieve, obtain composite ceramic material;
A2) by single functional group organism acrylamide and double-functional group organism linking agent N, N-methylene-bisacrylamide mixes according to mass ratio 100:1 ~ 10:1, be dissolved in deionized water and fully stir and obtain premixed liquid, wherein the content of acrylamide is 10～20%wt;
A3) composite ceramic material obtaining in step a1 and a2 is mixed according to volume ratio 40:60 ~ 65:35 with premixed liquid, be incorporated as in addition the ammonium citrate of composite ceramic material massfraction 0.1 ~ 2.5% as dispersion agent, ball milling 12 ~ 24h obtains the stable suspension of high solid loading, by ammoniacal liquor, regulate pH to 8 ~ 10.5, its viscosity is 0.5 ~ 2Pas;
A4) suspensoid step a3 being obtained is in whipping process, and dropwise adding successively cumulative volume is 0.2～1.0% catalyst n, N, N'N'-Tetramethyl Ethylene Diamine solution and 0.02～0.1% initiator ammonium persulfate, then vacuum outgas;
A5) slurry step a4 being obtained, injects rapidly the spherical cavity mould being comprised of upper and lower half module, and described alumina-ceramic hollow float external diameter is 40 ~ 300mm;
Wherein, in step a5, inject the amount of slurry and determine according to the shell thickness of required preparation Ceramic Balls, spherical cavity scribbles vacuum grease in advance as releasing agent;
A6) mould that slurry is housed in step a5 is carried out to all-directional rotation 5 ~ 10min, slurry is evenly attached on ball cavity wall, then in rotation, the temperature of mould is remained on to 55 ~ 75
oc realizes curing molding, obtains aluminum oxide green compact;
A7) by the aluminum oxide green compact that obtain in step a6 in temperature 50
oc, carries out predrying 72h under the environment of humidity 50%; Then 100
oin the baking oven of C, be dried 48h, fully slough the moisture of green compact, finally obtain dry alumina-ceramic hollow float green compact.
In step 3, described alumina-ceramic hollow float carries out sintering by non-pressure sintering technology, comprises the following steps:
B1) step a7 aluminum oxide green compact are positioned in retort furnace, under air atmosphere with 2
othe temperature rise rate of C/min rises to 300 ~ 800
obetween C, and be incubated 2h, fully the whole organism in burn off green compact;
B2), by alumina-ceramic hollow float after step b1 degumming technology, continue with 5
othe temperature rise rate of C/min rises to 1600 ~ 1800
obetween C, carry out sintering, and be incubated 1h, obtain fine and close alumina-ceramic hollow float sintered compact;
B3), alumina-ceramic hollow float sintered compact described in step b2 is carried out to surface strengthening and WATER REPELLENT.
In step b3, immersed 1 ~ 2s in the Glaze Slip being formed by silicate composite, made its surface adhesion one deck glaze, dry after 500 ~ 800
obetween C, heat, glaze fusing forms layer of transparent ceramic glaze layer and covers sintered compact surface, thick
Beneficial effect of the present invention:
Deep-sea proposed by the invention is withstand voltage alumina-ceramic hollow float and preparation method thereof, not only can provide larger buoyancy, and there is extremely strong ultimate compression strength, can tolerate the pressure of deep-sea 11000m, solve the unmanned bathyscaph of large degree of depth solid buoyancy material problem used, for ocean petroleum developing, there is important engineering significance and economic worth.
Embodiment
Below in conjunction with specific embodiment, the present invention is done to progressive explanation.Should be understood that following examples are only for the present invention is described but not for limiting scope of the present invention.
Embodiment 1 mixes 380 grams of aluminum oxide with 3.8 grams of magnesium oxide, be placed in 2L polyurethane ball-milling pot, adds the alumina-ceramic abrading-ball (768 grams) that doubles its quality, and 600ml spirituous solution, ball milling 24h post-drying, sieves, and obtains composite ceramic material.
Again 15 grams of acrylamides and 1.5 grams of N,N methylene bis acrylamides mixed and are dissolved in 95ml deionized water, fully stirring and obtain premixed liquid.Then composite ceramic is mixed with premixed liquid, and strong stirring, then add after 5 grams of ammonium citrates, ball milling 24h continued.Then add 0.5ml strong aqua that pH value is adjusted into 8, its viscosity is 0.9Pas.
Add again 0.5ml N, N, N'N'-Tetramethyl Ethylene Diamine solution and two ammonium persulfate solutions, inject rapidly the spherical cavity mould being comprised of upper and lower half module after vacuum outgas, and ball chamber diameter is 90mm.
Mould is carried out, after all-directional rotation 5min, the temperature of mould being remained on to 60 simultaneously
oc realizes curing molding, obtains aluminum oxide green compact.
Through after drying again 600
othe C 2h that comes unstuck, then 1800
oc sintering obtains fine and close sintered compact.Sintered compact is immersed in 1s in glaze slip the most at last, and 600
oc sintering 1h, the alumina-ceramic hollow float that acquisition shell thickness is 4mm.
Embodiment 2 mixes 217 grams of aluminum oxide with 10 grams of silicon oxide, be placed in 2L polyurethane ball-milling pot, adds the alumina-ceramic abrading-ball (454 grams) that doubles its quality, and 600ml spirituous solution, ball milling 24h post-drying, sieves, and obtains composite ceramic material.
In the present embodiment, aluminum oxide and silicon oxide are the compositions of common sintered alumina pottery, and the key of this patent is technique that its rotation gel injection obtains alumina-ceramic hollow ball.
Again 9 grams of acrylamides and 0.9 gram of N,N methylene bis acrylamide mixed and are dissolved in 90ml deionized water, fully stirring and obtain premixed liquid.Then composite ceramic is mixed with premixed liquid, and strong stirring, then add after 2 grams of ammonium citrates, ball milling 24h continued.Then add 0.6ml strong aqua that pH value is adjusted into 8.5, its viscosity is 0.5Pas.
Add again 0.6ml N, N, N'N'-Tetramethyl Ethylene Diamine solution and two ammonium persulfate solutions, inject rapidly the spherical cavity mould being comprised of upper and lower half module after vacuum outgas, and ball chamber diameter is 90mm.
Mould is carried out, after all-directional rotation 5min, the temperature of mould being remained on to 60 simultaneously
oc realizes curing molding, obtains aluminum oxide green compact.
Through after drying again 600
othe C 2h that comes unstuck, then 1650
oc sintering obtains fine and close sintered compact.Sintered compact is immersed in 1s in glaze slip the most at last, and 600
oc sintering 1h, the alumina-ceramic hollow float that acquisition shell thickness is 2.2mm.
Embodiment 3 mixes 37 grams of aluminum oxide with 1.5 grams of magnesium oxide, be placed in 1L polyurethane ball-milling pot, adds the alumina-ceramic abrading-ball (77 grams) that doubles its quality, and 200ml spirituous solution, ball milling 24h post-drying, sieves, and obtains composite ceramic material.
Again 1 gram of acrylamide and 0.02 gram of N,N methylene bis acrylamide mixed and be dissolved in 20ml deionized water, fully stirring and obtain premixed liquid.Then composite ceramic is mixed with premixed liquid, and strong stirring, then add after 0.4 gram of ammonium citrate, ball milling 24h continued.Then add 0.2ml strong aqua that pH value is adjusted into 9, its viscosity is 0.5Pas.
Add again 0.3ml N, N, N'N'-Tetramethyl Ethylene Diamine solution and an ammonium persulfate solution, inject rapidly the spherical cavity mould being comprised of upper and lower half module after vacuum outgas, and ball chamber diameter is 40mm.Mould is carried out, after all-directional rotation 5min, the temperature of mould being remained on to 60 simultaneously
oc realizes curing molding, obtains aluminum oxide green compact.
Through after drying again 600
othe C 1h that comes unstuck, then 1700
oc sintering obtains fine and close sintered compact.Sintered compact is immersed in 1s in glaze slip the most at last, and 600
oc sintering 1h, the alumina-ceramic hollow float that acquisition shell thickness is 2mm.
Above the specific embodiment of the present invention is illustrated, but the present invention is as limit, only otherwise depart from aim of the present invention, the present invention can also have various variations.
Claims (9)
1. the withstand voltage alumina-ceramic hollow float in deep-sea, is characterized in that, according to mass percent meter, its formula is:
Aluminum oxide 94% ~ 99.9% wt;
Sintering aid 0.1% ~ 6% wt.
2. alumina-ceramic hollow float according to claim 1, is characterized in that: described sintering aid is any one or combination of magnesium oxide, silicon oxide, and its total content is 0.1% ~ 6%wt.
3. alumina-ceramic hollow float according to claim 1, it is characterized in that: described alumina-ceramic hollow float external diameter is distributed in 40 ~ 300mm, the shell thickness of described alumina-ceramic hollow float is 2 ~ 12mm, and the shell thickness deviation of described alumina-ceramic hollow float is 0.1 ~ 2.5mm.
4. alumina-ceramic hollow float according to claim 1, is characterized in that: the maximum opposing of described hollow float hydrostaticpressure is 150MPa.
5. a preparation method for the withstand voltage alumina-ceramic hollow float in deep-sea as claimed in claim 1, is characterized in that, comprises the following steps:
Step 1, ready reaction raw material: aluminum oxide is mixed with sintering aid ball milling, acrylamide and linking agent N,N methylene bis acrylamide are dissolved in to the abundant acquisition premixed liquid that stirs in deionized water;
Step 2, rotation gel injection: by ceramic powder and premixed liquid mix and blend, add dispersion agent, catalyzer, initiator, after vacuum outgas, inject spherical cavity, by all-directional rotation, slurry is evenly attached on ball cavity wall, then control temperature and realize curing molding, after being dried, obtain aluminum oxide ball float green compact;
Step 3, come unstuck and sintering: by dry ceramic ball float base substrate 300 ~ 800
obetween C, heating is come unstuck, 1600 ~ 1800
obetween C, carry out sintering, obtain fine and close sintered compact;
Step 4, glazing: sintered compact is flooded in glaze slip, and 500 ~ 800
obetween C, heat, at its surface coverage layer of transparent ceramic glaze layer.
6. preparation method according to claim 5, is characterized in that: in step 2, described alumina-ceramic hollow float, by rotation gel injection technological forming, comprises the following steps:
A1) aluminum oxide and sintering aid are added in ball grinder, then add the alumina-ceramic abrading-ball that doubles its quality, by both ball millings in spirituous solution, it is evenly mixed, then dry, sieve, obtain composite ceramic material;
A2) by single functional group organism acrylamide and double-functional group organism linking agent N, N-methylene-bisacrylamide mixes according to mass ratio 100:1 ~ 10:1, be dissolved in deionized water and fully stir and obtain premixed liquid, wherein the content of acrylamide is 10～20%wt;
A3) composite ceramic material obtaining in step a1 and a2 is mixed according to volume ratio 40:60 ~ 65:35 with premixed liquid, be incorporated as in addition the ammonium citrate of composite ceramic material massfraction 0.1 ~ 2.5% as dispersion agent, ball milling 12 ~ 24h obtains the stable suspension of high solid loading, by ammoniacal liquor, regulate pH to 8 ~ 10.5, its viscosity is 0.5 ~ 2Pas;
A4) suspensoid step a3 being obtained is in whipping process, and dropwise adding successively cumulative volume is 0.2～1.0% catalyst n, N, N'N'-Tetramethyl Ethylene Diamine solution and 0.02～0.1% initiator ammonium persulfate, then vacuum outgas;
A5) slurry step a4 being obtained, injects rapidly the spherical cavity mould being comprised of upper and lower half module, and described alumina-ceramic hollow float external diameter is 40 ~ 300mm;
A6) mould that slurry is housed in step a5 is carried out to all-directional rotation 5 ~ 10min, slurry is evenly attached on ball cavity wall, then in rotation, the temperature of mould is remained on to 55 ~ 75
oc realizes curing molding, obtains aluminum oxide green compact;
A7) by the aluminum oxide green compact that obtain in step a6 in temperature 50
oc, carries out predrying 72h under the environment of humidity 50%; Then 100
oin the baking oven of C, be dried 48h, fully slough the moisture of green compact, finally obtain dry alumina-ceramic hollow float green compact.
7. preparation method according to claim 6, is characterized in that: in step a5, inject the amount of slurry and determine according to the shell thickness of required preparation Ceramic Balls, spherical cavity scribbles vacuum grease in advance as releasing agent.
8. preparation method according to claim 5, is characterized in that: in step 3, described alumina-ceramic hollow float carries out sintering by non-pressure sintering technology, comprises the following steps:
B1) step a7 aluminum oxide green compact are positioned in retort furnace, under air atmosphere with 2
othe temperature rise rate of C/min rises to 300 ~ 800
obetween C, and be incubated 2h, fully the whole organism in burn off green compact;
B2), by alumina-ceramic hollow float after step b1 degumming technology, continue with 5
othe temperature rise rate of C/min rises to 1600 ~ 1800
obetween C, carry out sintering, and be incubated 1h, obtain fine and close alumina-ceramic hollow float sintered compact;
B3), alumina-ceramic hollow float sintered compact described in step b2 is carried out to surface strengthening and WATER REPELLENT.
9. preparation method according to claim 8, is characterized in that: in step b3, immersed 1 ~ 2s in the Glaze Slip being formed by silicate composite, made its surface adhesion one deck glaze, dry after 500 ~ 800
obetween C, heat, glaze fusing forms layer of transparent ceramic glaze layer and covers sintered compact surface, and thickness is 0.05 ~ 0.15mm.
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