CN103896601B - Hot pressed sintering method of ceramic products with high density and complex shapes - Google Patents
Hot pressed sintering method of ceramic products with high density and complex shapes Download PDFInfo
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Abstract
The invention belongs to the technical field of preparation and forming methods of ceramic materials and in particular relates to a hot pressed sintering method of ceramic products with high density and complex shapes. In the method, a process for forming ceramic bodies with steel molds, which belongs to traditional hot pressed sintering processes, is abandoned. The method is characterized by firstly preparing a mold material into a required mold with a complex shape through a gel forming process, or firstly preparing a body of the mold material by adopting cold isostatic pressing, secondly machining the body into a required mold with a complex shape by adopting a numerically-controlled machine tool, thirdly preparing the target ceramic powder into slurry with high solid content by adopting the advanced gel forming technology, and injecting the slurry into the mold to form the composite hot-pressed body; or firstly preparing the target ceramic powder into a part body through a gel casting process, secondly injecting the mold material slurry through the gel casting technology to form the composite hot-pressed body, and removing the hot-pressed mold material after sintering, thus finally obtaining the ceramic products with complex structures and high density and properties.
Description
Technical field
The invention belongs to stupalith and prepare shaping method and technology field, particularly a kind of hot-pressing sintering method of high-compactness complicated shape ceramic.
Background technology
Hot-pressing sintering technique is one of sintering process that pottery or Powder Metallurgy Industry are conventional, its basic procedure is, first will the ceramic powder of sintering be needed to pour in steel die, the ceramic body of formation about 35% ~ 40% theoretical density is made it with certain pressure, then this base substrate is loaded in previously prepd high strength graphite mould, and put it in hot-pressed sintering furnace, by high-strength graphite pressure head, heat while pressurize, at high temperature, the high-compactness sintering of ceramic powder is realized under high pressure, in actual production, also the normal graphite jig that directly loaded by ceramic powder sinters, Fig. 1 is SiC ceramic hot pressed sintering schematic diagram.Compared with ordinary sinter, the advantage of hot pressed sintering: 1. there is obvious Grain Boundary Sliding mass transfer and extruding creep mass transfer, sintering rate is accelerated, and firing time reduces; 2. can reduce sintering temperature, reduce grain growth; 3. the density of the finished product and mechanical property high.Table 1 is the SiC ceramic performance comparison of different methods sintering, it can thus be appreciated that hot pressed sintering is the most effective way preparing high-compactness silicon carbide ceramics.
But well-known, hot-pressing sintering technique also has obvious shortcoming, the impact by processing method usually can only the simple goods of sintered shape, and as the ceramic product of tabular class, the block class of square, cylindric type, thus its range of application is also subject to serious restriction.Along with the fast development of science and technology, every profession and trade gets more and more to the demand of high-compactness, complicated shape ceramic, although adopt cold isostatic compaction+forming technique such as mechanical workout or gel injection and non-pressure sintering technology can obtain the ceramic component of complicated shape, but the requirement that cannot meet under many circumstances ceramic component high-compactness, and the pressureless sintering of complicated shape ceramic component needs slow and meticulous temperature control technique, long high temperature sintering can impel grain growth, reduces the mechanical property of ceramic part.If adopt post-hiped technology to improve the density of pressureless sintering base substrate, greatly manufacturing cost can be increased.
The object of the present invention is to provide the hot-pressing production process of a kind of high densification, complicated shape ceramic, by hot pressed sintering ceramic technology of the present invention, the present situation that above-mentioned conventional thermocompression can only manufacture the ceramic product of simple tabular class can be overcome, the ceramic product with complex construction, high-compactness can be produced.
Summary of the invention
The present invention utilizes BN pottery to wait moulding stock target pottery of at high temperature getting along well that the characteristic of chemical reaction occurs, moulding stock and target stupalith is made to realize synchronous at high temperature under high pressure by the formula adjusting moulding stock, guarantee that the complicated shape of target pottery is retained, this is technical essential of the present invention.The technique of traditional steel die forming ceramic base substrate is abandoned in this invention, by the present invention, can prepare the ceramic of high-compactness, complicated shape.
Not enough for prior art, the invention provides a kind of hot-pressing sintering method of high-compactness complicated shape ceramic.
A kind of hot-pressing sintering method of high-compactness complicated shape ceramic, first moulding stock is prepared into the required mould with specified shape by gel forming technique, then the target ceramic powder employing gel forming technology needing to sinter is prepared into the slurry containing solid-phase component, injects in above-mentioned mould and form compound thermal pressed compact body; Gained compound thermal pressed compact body is by removing residual moulding stock after hot pressed sintering, final acquisition has the target ceramic of specific structure, density, performance.
Described moulding stock is not reacted with target stupalith and can be processed by machinery or chemical process and removes under sintering condition.
Described moulding stock is BN, the matrix material of BN and SiC, BN and Al
2o
3matrix material, BN and Si
3n
4matrix material, the matrix material of BN and other potteries, graphite or graphite and pottery matrix material.
Describedly moulding stock is prepared into the required concrete grammar with the mould of specified shape by gel forming technique is: selected moulding stock powder is prepared into slurry by gel forming technique; According to the shape and size of the ceramic part that will sinter, consider the shrinking percentage in process redundancy and hot pressing direction, adopt mechanical workout or 3D printing technique to prepare plastics that core mates with part shape or metal die; Described plastics or metal die inner cavity size should close with hot pressing die inner sleeve matching size; The moulding stock slurry prepared is injected in the plastics or metal die processed, is heated to 60 DEG C ~ 80 DEG C, constant temperature certain hour until its gel solidification is shaping, take out core rod obtain needed for there is specified shape, the mould prepared by moulding stock;
Or adopt isostatic cool pressing method first to prepare moulding stock base substrate, then be processed into the mould of desired shape by numerically-controlled machine.
Described target ceramic powder is SiC, Si
3n
4, AlN, AlON, the ceramic powder material of aluminum oxide or zirconium white etc. or composite powder material.
After described compound thermal pressed compact body integral heat pressure sintering, remove residual moulding stock by blasting craft, final acquisition has the target ceramic of ad hoc structure, density, performance.
Technical characteristic of the present invention is:
A. select and the moulding stock needing the target stupalith sintered that chemical reaction does not at high temperature occur, should remove easily through machinery or chemical process after this moulding stock sintering, matrix material, BN and the Al of BN, BN and SiC can be selected
2o
3matrix material, BN and Si
3n
4matrix material, graphite or graphite and pottery matrix material etc. as moulding stock.
B. selected moulding stock powder is prepared into slurry by gel forming technique.
C. according to the shape and size of the ceramic part that will sinter, consider the shrinking percentage in certain process redundancy and hot pressing direction, adopt mechanical workout or 3D printing technique to prepare the core plastics similar to part shape or metal die.These plastics or metal die inner cavity size should close with hot pressing graphite jig inner sleeve matching size.
D. by the plastics processed in the moulding stock slurry implantation step c prepared in step b or metal die, be heated to 60 DEG C ~ 80 DEG C, it is shaping that constant temperature certain hour makes it gel solidification, take out core rod obtain needed for there is complicated shape, the mould prepared by moulding stock.
E. target ceramic powder (SiC, Si of sintering will be needed
3n
4, aluminum oxide or Zirconium powder material etc.) adopt advanced gel forming technology to be prepared into the slurry of high solid loading, inject in above-mentioned mould, after gel solidification, form compound thermal pressed compact body.
F. load in hot pressing graphite jig by the compound thermal pressed compact body obtained in step e, after integral heat pressure sintering, remove aforesaid moulding stock by blasting craft, final acquisition has complex construction, high-density, high performance target ceramic.
In above-mentioned technical characteristic, moulding stock is also by the mould described in cold isostatic compaction and mechanical workout preparation process d.
Technical characteristic of the present invention, also first can prepare the gel grout material of target ceramic powder, according to the technology processing plastic identical with step c or metal die, these plastics or metal die inner chamber similar to part shape.By the target ceramic powder gel grout material injected plastic prepared or metal die, and gel forming; Then as core, moulding stock gel note technique is poured into periphery, the compound thermal pressed compact body described in forming step e.
Beneficial effect of the present invention is:
The inventive method takes full advantage of the technical characterstic of gel note technique and heat pressing process, and providing one can prepare complicated shape, and can stablize again the hot pressing production technology obtaining high-compactness ceramic, be the innovation of conventional thermocompression technique.
Accompanying drawing explanation
Fig. 1 is SiC ceramic hot pressed sintering schematic diagram;
1-1 wherein in Fig. 1 is the seaming chuck of the band water-cooling structure that high temperature steel is made, and plays the effect of the SiC ceramic transmission of pressure to hot pressing; 1-2 is graphite seaming chuck, plays the effect of direct pressing SiC ceramic; 1-3 is the SiC ceramic receiving hot pressing; 1-4 is graphite push-down head, acts on identical with 1-2; 1-5 is graphite overcoat, plays the effect of constraint hot pressing SiC ceramic; 1-6 is graphite heater, plays the effect of heating SiC ceramic; 1-7 is the push-down head of the band water-cooling structure that high temperature steel is made, and acts on identical with 1-1.
Fig. 2 is the embodiment of the present invention 1 gel casting SiC and BN preparation technology schema;
Fig. 3 is the aluminium alloy jacket structure schematic diagram of casting mold material and target pottery, and wherein Fig. 3 a is the front view of aluminum alloy outer frame, and Fig. 3 b is the vertical view of aluminum alloy outer frame;
Fig. 4 is SiC ceramic upper mold core structural representation (using for during gel mold target forming process of ceramics), and wherein Fig. 4 a is the front view of SiC ceramic upper mold core, and Fig. 4 b is the sectional view (A-A face have rotated 180 degree) of SiC ceramic upper mold core;
Fig. 5 is SiC ceramic lower mold core structural representation (using for during gel mold target forming process of ceramics), and wherein Fig. 5 a is the vertical view of SiC ceramic lower mold core, and Fig. 5 b is the front view of SiC ceramic lower mold core;
Fig. 6 is mould material BN seaming chuck or push-down head structural representation, and wherein Fig. 6 a is the vertical view of BN seaming chuck or push-down head, and Fig. 6 b is the front view of BN seaming chuck or push-down head;
Fig. 7 is SiC and the BN plural gel body structure schematic diagram after gel drying, wherein Fig. 7 a is the vertical view of SiC and BN plural gel body, Fig. 7 b is the main pseudosection of SiC and BN plural gel body (B-B face), 7-1 in figure is moulding stock BN, 7-2 is that target material SiC, 7-3 are for being moulding stock BN;
Fig. 8 is the SiC product structure schematic diagram of the complex section completed in example of the present invention; Wherein Fig. 8 a is the vertical view of SiC product, and Fig. 8 b is the main pseudosection (C-C face) of SiC product.
Embodiment
The invention provides a kind of hot-pressing sintering method of high-compactness complicated shape ceramic, below in conjunction with the drawings and specific embodiments, the present invention will be further described.
Embodiment 1
Gel casts preparation technology's flow process of SiC and BN as shown in Figure 2:
The processing step preparing gel casting SiC ceramic and BN pottery is as follows:
(1) monomer solution is configured:
Acrylamide (AM) monomer and linking agent methylene-bisacrylamide (MBAM) are prepared to be dissolved in deionized water by a certain percentage and prepares monomer solution; Wherein in monomer solution containing AM be 11.4wt%, be 1wt% containing MBAM, containing pure water 87.6wt%.The monomer solution prepared is dissolved fully, stand-by with being enclosed in after filter paper filtering in Glass Containers.
(2) dispersant solution is configured:
In 10g citric acid ammonia (DAC)+90g water ratio by citric acid ammonia (DAC) and water mixed dissolution fully after, the dispersion agent liquid prepared is dissolved fully, stand-by with being enclosed in after filter paper filtering in Glass Containers.
(3) batch mixing:
A. weigh in the balance and get 5kg zirconium oxide balls, the diameter of zirconia ball is Φ 6mm, puts into the vertical mixing mill that volume is 5L;
B. two parts of 720g monomer solutions are measured with the gentle transfer pipet in sky;
C. two parts of 40ml dispersion agents are measured with the gentle dropper in sky;
D. minute quantity defrother is added; (add 0.05% defrother accounting for monomer solution weight, what add in this example is dimethyl-silicon oil hydrosol, and its oleaginousness is 30%)
E. weigh 2.304kg SiC powder and 1.584kg BN powder respectively, join respectively in the monomer liquid of the different 720g previously prepared.Now the volumetric concentration of SiC and BN monomer solution is all 50vol%.（2304/3.2=720cm
3）（1.584/2.2=720cm
3）。Wherein the theoretical density of SiC ceramic is ρ
siC=3.2(g/cm
3), the theoretical density of BN pottery is ρ
bN=2.2(g/cm
3);
F. respectively stirring ball-milling 4h is carried out to SiC and BN monomer slurry, slurry is uniformly dispersed.
(4) slip process:
The monomer slurry stirred (SiC monomer slurry or BN monomer slurry) is filtered out mill with 150 eye mesh screens be respectively situated between and impurity, with stand-by inside the refrigerator being kept at 0 DEG C after Plastic Bottle or vial sealing.
(5) casting die mould prepares:
Adopt cast aluminium as the die casting instrument of slurry, comprise overcoat (see figure 3), up and down core rod (see Fig. 4,5,6), wherein core rod is divided into two covers, and a set of has been complex section core rod, completed by mechanical workout or 3D printing technique, another set of is dull and stereotyped core rod, adopts mechanical workout to complete, ensures that the load face of shaping colloid is smooth.
(6) process of casting SiC slurries:
Except the air in slurry, the upper mold core of press-in, until discharge without gas in slurry, contacts completely with slurry, SiC monomer syrup is taken out 400g from refrigerator, add ammonium persulphate 3g ~ 4g, with magnetic stirrer evenly after (according to slurry number, period and temperature as far as possible, avoid slurry before injection mould, there is gel reaction) pour in preprepared cast-aluminum die, wherein up and down core rod adopts core rod with complex section (see Fig. 4, 5), first the lower mold core (Fig. 5) of band complex section is put into cast aluminium die sleeve (Fig. 3), then band initiator is poured into---the SiC monomer slurry of ammonium persulphate, by the upper mold core (Fig. 4) of band complex section manually, be pressed into gently in cast aluminium die sleeve (Fig. 3), upper mold core is with exhaust structure passage, be convenient to get rid of the gas in mould.
(7) Gel Treatment of SiC slurry:
SiC slurry cast-aluminum die in aluminum dipping form is together put into the drying baker of 80 DEG C, at 80 DEG C of temperature, after placing 30min, take out cast-aluminum die, take out upper mold core (Fig. 4), check the gel state of SiC slurry, SiC colloid is touched, if there is elasticity and do not deform with finger.
(8) process of BN monomer slurry and mold:
Repeat (6) operation steps, SiC slurry is changed into BN slurry, upper and lower core rod is replaced with dull and stereotyped core rod (Fig. 6), by BN slurry 100g, inject cast-aluminum die, make BN slurry be full of on the SiC colloid of gel, upper and lower for flat board core rod (Fig. 6) is pressed in cast aluminium die sleeve (Fig. 3) successively, until dull and stereotyped core rod (Fig. 6) touches BN slurry.Put into the gelation process 30min that drying baker (temperature of drying baker is arranged on 60 ~ 80 DEG C) does BN slurry again.
(9) drying and processing:
By SiC and BN plural gel body good for gel, deviate from from cast-aluminum die, be placed on indoor and dry in the shade without the place of direct sunlight, ambient temperature controls within the scope of 10 ~ 25 DEG C, too high temperature may cause blank cracking, the composite body dried in the shade, and can load next step hot pressing process.
Hot-pressing sintering technique step:
(1) dried SiC and BN plural gel body (see figure 7), adopt conventional SiC heat pressing process, load in graphite jig, the sintering of SiC and BN plural gel body can be completed.
(2) hot pressed sintering of SiC and BN plural gel body and single SiC hot pressed sintering difference are, SiC is required product material, BN is the shape needs ensureing SiC the finished product, and bi-material, in hot pressed sintering process, remains synchronous sintering shrinkage state.
The process of later stage SiC and BN composite sinter:
(1) by SiC and BN complex body good for hot pressed sintering, grind two large faces by surface grinding machine, that is, the carbon paper be attached in sintering process above sintered compact is ground off, expose the BN material at two ends.
(2) by SiC and the BN composite sinter of completing steps (1), with the spray gun of sand-blasting machine of pressure 0.2Mpa ~ 1Mpa, based on 80-150 object SiC steel sand, carrier is done with water, the process of removing BN is carried out to it, because BN and SiC is in high temperature hot pressing sintering, there is not chemical reaction, be therefore easy to just can also remove from complex body.The hot pressed sintering body of SiC complex section as shown in Figure 8.
(3) by the only remaining SiC hot pressed sintering material presenting complex construction of completing steps (2), can carry out necessary mechanical workout as required, a satisfactory ceramic product with the SiC hot pressed sintering of the densification of complex construction, has just produced.
The thyrite physical property data table of table 1 different sintering processes
Embodiment 2
Hot pressing target pottery Si
3n
4, using C powder and BN as moulding stock:
(1) first according to the processing step of example 1, configuration Si
3n
4slurry, and with die coat (Fig. 3), seaming chuck (Fig. 4), push-down head (Fig. 5) gel forming Si
3n
4slurry;
(2) using C powder and BN mixture as moulding stock, wherein the massfraction of C powder is the massfraction of 80%, BN is 20%, utilizes isostatic cool pressing, goes out block at the forming under the pressure of 200MPa, adopts CNC milling machine to process and Si
3n
4the shape and size that gelinite top and bottom coincide;
(3) by the C powder that processes and BN mixture moulding stock and Si
3n
4gelinite assembling is worked good, and by heat pressing process and the aftertreatment technology of example 1, can complete the Si with complex construction
3n
4the manufacture of ceramic product.
The explanation of nouns of relevant technical terms
1, hot pressed sintering (Hot Pressed Sintering):
The ceramic powder of drying is filled in model, adds flanging heating by unidirectional or two-way limit, make shaping and sinter a kind of ceramic post sintering method simultaneously completed.
2, SiC ceramic:
With the pottery that silicon carbide (SiC) is main component.
3, high-strength graphite:
One has high-density, high strength, high temperature mechanical strength, high density/weight ratio and the graphite material of anti-thermal shock quality.
4、HRA：
The A scale of Rockwell hardness is represented in Rockwell hardness.
5, gel forming technique:
By preparing the slurry of high solid volume fraction of low-viscosity, high workability, then the organic monomer polymerization in slurry is made slurry solidify in place, thus obtain the base substrate of high-density, high strength, good uniformity.
6, acrylamide (AM):
Acrylamide (AM) is a kind of white crystal chemical substance, water-soluble, as monomer component in gel process.
7, methylene-bisacrylamide (MBAM):
Water-soluble white organic materials, as crosslinker component in gel process.
8, citric acid ammonia (DAC):
White deliquescence powder or crystallization, soluble in water, the composition undertaking dispersion agent in gel process exists, and ensures the dispersion of ceramic particle and does not reunite.
Claims (5)
1. the hot-pressing sintering method of a high-compactness complicated shape ceramic, it is characterized in that: first moulding stock is prepared into the required mould with specified shape by gel forming technique, then the target ceramic powder employing gel forming technology needing to sinter is prepared into the slurry containing solid-phase component, injects in above-mentioned mould and form compound thermal pressed compact body; Gained compound thermal pressed compact body is by removing residual moulding stock after hot pressed sintering, final acquisition has the target ceramic of specific structure, density, performance;
Described moulding stock is not reacted with target ceramic powder and can be processed by machinery or chemical process and removes under sintering condition.
2. the hot-pressing sintering method of a kind of high-compactness complicated shape ceramic according to claim 1, is characterized in that: described moulding stock is BN material.
3. the hot-pressing sintering method of a kind of high-compactness complicated shape ceramic according to claim 1, it is characterized in that, describedly moulding stock is prepared into the required concrete grammar with the mould of specified shape by gel forming technique is: selected moulding stock powder is prepared into slurry by gel forming technique; According to the shape and size of the ceramic part that will sinter, consider the shrinking percentage in process redundancy and hot pressing direction, adopt mechanical workout or 3D printing technique to prepare plastics that core mates with part shape or metal die; Described plastics or metal die inner cavity size should close with hot pressing die inner sleeve matching size; The moulding stock slurry prepared is injected in the plastics or metal die processed, is heated to 60 DEG C ~ 80 DEG C, constant temperature certain hour until its gel solidification is shaping, take out core rod obtain needed for there is specified shape, the mould prepared by moulding stock.
4. the hot-pressing sintering method of a kind of high-compactness complicated shape ceramic according to claim 1, is characterized in that: described target ceramic powder is SiC, Si
3n
4, AlN, AlON, aluminum oxide or zirconic ceramic powder material or composite powder material.
5. the hot-pressing sintering method of a kind of high-compactness complicated shape ceramic according to claim 1, it is characterized in that: after described compound thermal pressed compact body integral heat pressure sintering, remove residual moulding stock by blasting craft, final acquisition has the target ceramic of ad hoc structure, density, performance.
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| CN104496480B (en) * | 2014-12-08 | 2017-07-25 | 中国建筑材料科学研究总院 | Silicon carbide ceramics precast body, aluminum-base silicon carbide ceramic material and preparation method thereof |
| CN104788102B (en) * | 2015-03-23 | 2017-04-19 | 济南大学 | Preparation method for nano-silicon nitride powder for laser sintering 3D printing technology |
| US20180009032A1 (en) * | 2016-07-08 | 2018-01-11 | General Electric Company | Metal objects and methods for making metal objects using disposable molds |
| CN106735186B (en) * | 2016-12-07 | 2018-11-27 | 北京科技大学 | A kind of method that 3D printing-isostatic cool pressing prepares titanium alloy multi-stage gear |
| US20180251406A1 (en) * | 2017-03-06 | 2018-09-06 | Applied Materials, Inc. | Sintered ceramic protective layer formed by hot pressing |
| CN107840656B (en) * | 2017-10-30 | 2020-09-01 | 武汉理工大学 | Manufacturing method of 3D printing/gel casting composite forming zirconia full-porcelain tooth |
| CN108995014B (en) * | 2018-03-26 | 2023-08-15 | 吉林大学 | Spiral tube type ceramic blank preparation mold and method |
| CN109016082B (en) * | 2018-09-21 | 2020-06-23 | 王雨婷 | Full-automatic ceramic hot press |
| CN109413783B (en) * | 2018-11-23 | 2021-07-30 | 福建闽航电子有限公司 | Manufacturing method of ceramic heating device for intelligent closestool |
| CN112140282B (en) * | 2020-09-28 | 2022-02-15 | 中航装甲科技有限公司 | Method for improving fluidity of silicon-based ceramic core slurry |
| CN112299856B (en) * | 2020-11-16 | 2022-04-22 | 中国工程物理研究院材料研究所 | AlON ceramic powder preparation method based on 3D printing forming |
| CN112919915B (en) * | 2021-03-09 | 2022-12-02 | 南京理工大学 | Method for pressing silicon nitride ceramic special-shaped cutter by SPS pressure sintering powder |
| CN115194919A (en) * | 2022-08-02 | 2022-10-18 | 北京理工大学唐山研究院 | Mold for preparing AlON transparent ceramic by SPS (semi-permeable plasma sintering), preparation method and obtained transparent ceramic |
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| JPS6029674B2 (en) * | 1983-06-02 | 1985-07-11 | 科学技術庁無機材質研究所長 | Manufacturing method of high-density sintered body |
| KR0139551B1 (en) * | 1996-04-19 | 1998-06-01 | 우덕창 | Proce ss for simultaneously producing a number of ceramic sintered body by hot pressing method |
| JP2000272974A (en) * | 1999-03-24 | 2000-10-03 | Tdk Corp | Hot pressing and apparatus for hot pressing |
| JP2001240476A (en) * | 2000-02-28 | 2001-09-04 | Tdk Corp | Hot press method and manufacturing method of ceramic element |
| CN101747071A (en) * | 2009-12-15 | 2010-06-23 | 王占双 | Preparation of carbon/carbon mould for hot-pressed sintering furnace |
| CN102060555A (en) * | 2010-11-24 | 2011-05-18 | 西安超码科技有限公司 | Method for manufacturing high-strength carbon/carbon hot-press die |
| CN201999864U (en) * | 2011-01-06 | 2011-10-05 | 成都超纯应用材料有限责任公司 | Multilevel graphite mould for vacuum hotpressing furnace |
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