CN116143516B - High-purity stable-phase gamma-yttrium disilicate ceramic powder and preparation method thereof - Google Patents
High-purity stable-phase gamma-yttrium disilicate ceramic powder and preparation method thereof Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 86
- 239000000919 ceramic Substances 0.000 title claims abstract description 40
- 229910052727 yttrium Inorganic materials 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 26
- 238000000498 ball milling Methods 0.000 claims abstract description 19
- 238000002156 mixing Methods 0.000 claims abstract description 19
- 238000001035 drying Methods 0.000 claims abstract description 13
- 239000002243 precursor Substances 0.000 claims abstract description 10
- 238000002490 spark plasma sintering Methods 0.000 claims abstract description 10
- 238000007873 sieving Methods 0.000 claims abstract description 7
- 239000012298 atmosphere Substances 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 230000001681 protective effect Effects 0.000 claims abstract description 5
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 18
- 238000005245 sintering Methods 0.000 claims description 17
- 239000002245 particle Substances 0.000 claims description 15
- 239000002105 nanoparticle Substances 0.000 claims description 14
- 239000011268 mixed slurry Substances 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000004321 preservation Methods 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 229910021486 amorphous silicon dioxide Inorganic materials 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 230000000630 rising effect Effects 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 7
- 239000013078 crystal Substances 0.000 abstract description 4
- 230000035484 reaction time Effects 0.000 abstract description 2
- 239000003963 antioxidant agent Substances 0.000 abstract 1
- 230000003078 antioxidant effect Effects 0.000 abstract 1
- 239000012780 transparent material Substances 0.000 abstract 1
- 239000012071 phase Substances 0.000 description 32
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 25
- 238000006243 chemical reaction Methods 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 12
- 239000000463 material Substances 0.000 description 9
- 239000002994 raw material Substances 0.000 description 6
- 239000000243 solution Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000001027 hydrothermal synthesis Methods 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 238000003980 solgel method Methods 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 230000004913 activation Effects 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 239000006184 cosolvent Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 239000011363 dried mixture Substances 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910018557 Si O Inorganic materials 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 229910004283 SiO 4 Inorganic materials 0.000 description 1
- XEDZPTDJMMNSIB-UHFFFAOYSA-N [Si]([O-])([O-])([O-])O.[Y+3] Chemical compound [Si]([O-])([O-])([O-])O.[Y+3] XEDZPTDJMMNSIB-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000005234 chemical deposition Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005685 electric field effect Effects 0.000 description 1
- 238000000724 energy-dispersive X-ray spectrum Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000010587 phase diagram Methods 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- AKTQKAXQEMMCIF-UHFFFAOYSA-N trioxido(trioxidosilyloxy)silane;yttrium(3+) Chemical compound [Y+3].[Y+3].[O-][Si]([O-])([O-])O[Si]([O-])([O-])[O-] AKTQKAXQEMMCIF-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses high-purity stable phase gamma-yttrium disilicate ceramic powder and a preparation method thereof, wherein the preparation method comprises the following steps: will be nano-scale Y 2 O 3 Adding the powder and the silica sol into water, ball-milling and mixing, drying, crushing and sieving to obtain precursor powder; and (3) performing spark plasma sintering on the obtained precursor powder under the condition of protective atmosphere or vacuum or no mechanical pressure, and then naturally cooling to obtain the high-purity stable-phase gamma-yttrium disilicate ceramic powder. The preparation method has the advantages of short reaction time, simple equipment, safe process and low cost, and the obtained gamma-yttrium disilicate ceramic powder has high purity and stable crystal structure, and has wide application prospect in the field of high-temperature-resistant antioxidant wave-transparent materials.
Description
Technical Field
The invention relates to the technical field of preparation of high-temperature-resistant and oxidation-resistant ceramic powder, in particular to a preparation method of high-purity stable-phase gamma-yttrium disilicate ceramic powder.
Background
Y-Si-O ceramics having complex polytype phases, yttrium monosilicate Y 2 SiO 5 There are two polytype phases (X1 and X2), yttrium disilicate Y 2 Si 2 O 7 There are 7 polytype phases (Y, α, β, γ, δ, ζ and η) which undergo interconversion with temperature and pressure changes, wherein X2-Y 2 SiO 5 And gamma-Y 2 Si 2 O 7 The two ceramic materials have high temperature phases with the most stable corresponding polytype phases, the melting points of the two phases are higher than 1950 ℃ and 1775 ℃, and the two ceramic materials have high resistanceThe material has excellent performances of oxidation, low thermal conductivity, low thermal expansion, low dielectric constant, high temperature resistance, chemical corrosion resistance and the like, so that the material is mainly applied to the fields of high-temperature oxidation-resistant coating materials, optical matrix materials, dielectric materials and the like, and is a high-temperature wave-transmitting material with great potential.
Y 2 SiO 5 And Y 2 Si 2 O 7 Initially at Y 2 O 3 And Y 2 O 3 /SiO 2 The silicon nitride ceramic grain boundary as sintering aid is found in Y 2 O 3 -SiO 2 In the reaction phase diagram, gamma-Y 2 Si 2 O 7 Only a very narrow region, thus synthesizing pure phase gamma-Y 2 Si 2 O 7 The powder is very difficult to use Y 2 O 3 And SiO 2 When the powder is used as a raw material, the conventional solid phase reaction method is generally difficult to synthesize, the powder can be prepared by heat preservation for 100 hours at the high temperature of 2100 ℃, repeated calcination and grinding are needed, and the preparation process is complex and has high cost. In addition, synthesis of Y has been reported 2 Si 2 O 7 The method mainly comprises a sol-gel method, a hydrothermal method, a microwave hydrothermal method, a sonochemical method, a laser chemical deposition method and the like, wherein the methods show different characteristics according to different applications, but have some defects, such as the sol-gel method needs to be added with a cosolvent to reduce the reaction temperature, the sol-gel process needs to be controlled by setting a staged temperature, the process is complex, and the added cosolvent has influence on the dielectric property of the powder; the hydrothermal method needs a long time of 24-200 hours to obtain; the sonochemistry method is obtained by generating local high temperature and high pressure in a reaction system by utilizing ultrasonic waves, and has strict requirements on reaction conditions. Therefore, there is a need to develop new methods for rapid synthesis of gamma-Y 2 Si 2 O 7 Ceramic powder.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects of the prior art and providing the high-purity stable-phase gamma-yttrium disilicate ceramic powder with high purity, short reaction time and stable crystal structure and the preparation method thereof.
In order to solve the technical problems, the invention adopts the following technical scheme.
The preparation method of the high-purity stable phase gamma-yttrium disilicate ceramic powder comprises the following steps:
s1, nanometer Y 2 O 3 Adding the powder and the silica sol into water, ball-milling and mixing to obtain mixed slurry, drying, crushing and sieving to obtain precursor powder; wherein the silica sol contains SiO 2 Aqueous solutions of nanoparticles, siO 2 Is amorphous SiO 2 The nanometer level Y 2 O 3 Powder and SiO in the silica sol 2 The mol ratio of (2) is 1:2.1-2.3;
s2, carrying out spark plasma sintering on the obtained precursor powder under the condition of protective atmosphere or vacuum or no mechanical pressure, and then naturally cooling to obtain the high-purity stable-phase gamma-yttrium disilicate ceramic powder, wherein the purity of the gamma-yttrium disilicate is more than 95%.
In the above method for preparing high-purity stable phase gamma-yttrium disilicate ceramic powder, preferably, in step S1, the nano-scale Y 2 O 3 Powder and SiO in the silica sol 2 The molar ratio of the mixed slurry is 1:2.15-2.25, and the solid content of the mixed slurry is 30-60 wt.%.
In the above method for preparing high-purity stable phase gamma-yttrium disilicate ceramic powder, preferably, in step S1, the nano-scale Y 2 O 3 The purity of the powder is more than or equal to 99.99 percent, and the grain diameter is 5nm to 50nm; the solid content of the silica sol is 20wt.% to 40wt.%, the pH value is 2 to 3, and the SiO in the silica sol 2 The particle diameter of the nano particles is 1 nm-10 nm.
In the above method for preparing high-purity stable phase gamma-yttrium disilicate ceramic powder, more preferably, in step S1, the nano-scale Y 2 O 3 The particle size of the powder is 5 nm-10 nm; siO in the silica sol 2 The particle diameter of the nano particles is 1 nm-3 nm.
In the preparation method of the high-purity stable phase gamma-yttrium disilicate ceramic powder, preferably, in the step S1, the ball milling and mixing time is 2-8 hours, and the rotational speed of the ball milling and mixing is 200-500 rpm; the drying temperature is 60-150 ℃, and the drying time is 8-24 hours; the rotational speed adopted for crushing is 2-3 ten thousand rpm, and the mesh number of the sieving is 500-5000 meshes.
In the preparation method of the high-purity stable phase gamma-yttrium disilicate ceramic powder, more preferably, in the step S1, the ball milling and mixing time is 4-6 hours, and the rotational speed of the ball milling and mixing is 300-400 rpm; the drying temperature is 80-100 ℃, and the drying time is 12-16 h; the mesh number of the sieve is 1000-2000 meshes.
In the preparation method of the high-purity stable phase gamma-yttrium disilicate ceramic powder, preferably, in the step S2, the heating rate of spark plasma sintering is 50 ℃/min-300 ℃/min, the sintering temperature is 1450-1600 ℃ and the heat preservation time is 1 min-10 min.
In the preparation method of the high-purity stable phase gamma-yttrium disilicate ceramic powder, preferably, in the step S2, the heating rate of spark plasma sintering is 100 ℃/min-150 ℃/min, the sintering temperature is 1500 ℃ -1560 ℃ and the heat preservation time is 3 min-6 min.
In the above preparation method of high-purity stable phase γ -yttrium disilicate ceramic powder, preferably, in step S2, the protective atmosphere is one or more of nitrogen, helium and argon.
As a general technical conception, the invention also provides the high-purity stable-phase gamma-yttrium disilicate ceramic powder prepared by the preparation method.
Compared with the prior art, the invention has the advantages that:
1. the invention selects nano Y 2 O 3 SiO in powder and silica sol 2 The nanometer particles are used as reaction raw materials, the nanometer particles in the silica sol have small particle size, are uniformly dispersed and are matched with nanometer Y 2 O 3 Can be fully and uniformly mixed during powder ball milling and mixing, and SiO 2 The nano particles are of isotropic amorphous structures, the specific surface area of the nano particles is large, a higher contact area is provided for reactants, the synthetic activation energy and the reaction temperature are reduced, the reaction degree of the nano particles and the reaction temperature is higher, and the reactants do not contain other metal ions such as doping auxiliary agents, so that the obtained product has higher purity and cannot be influencedDielectric properties of the sound powder.
2. The invention adopts the discharge plasma calcination method to synthesize the powder, can utilize the Joule heating effect and the electric field effect of strong pulse current to heat the material at high speed based on the discharge plasma sintering equipment, and has the advantages of rapid heating, rapid heat transfer, rapid heating rate and the like compared with the traditional process. The method of the invention generates discharge among particles to realize local pre-melting, has lower sintering temperature, accelerates atomic diffusion due to the activation of powder, has short sintering time, can finish the sintering process in a few minutes or more than ten minutes generally, has high efficiency, can control the grain growth and the microstructure of materials, can promote the rapid synthesis of ceramic powder, and greatly reduces the cost and the technological process.
3. The synthesized gamma-Y of the invention 2 Si 2 O 7 The ceramic powder has high purity, consists of a single phase, has stable crystal structure, is characterized by high temperature resistance, oxidation resistance, hot corrosion resistance, smaller thermal conductivity and thermal expansion coefficient, better dielectric constant and dielectric loss, and has wide application prospect in the field of high-temperature wave-transmitting materials.
Drawings
FIG. 1 shows a gamma-Y obtained in example 1 of the present invention 2 Si 2 O 7 XRD spectrum of ceramic powder.
FIG. 2 shows a gamma-Y obtained in example 1 of the present invention 2 Si 2 O 7 SEM photograph of ceramic powder.
FIG. 3 shows a gamma-Y obtained in example 1 of the present invention 2 Si 2 O 7 EDS spectrum of ceramic powder.
Detailed Description
The invention is further described below in connection with the drawings and the specific preferred embodiments, but the scope of protection of the invention is not limited thereby. The materials and instruments used in the examples below are all commercially available. The silica sol contains SiO 2 The aqueous solution of nanoparticles was purchased from xuan city, jinrui new materials limited.
Example 1
The preparation method of the high-purity stable phase gamma-yttrium disilicate ceramic powder comprises the following steps:
s1, 67.8g of nanoscale Y 2 O 3 Adding 50g of deionized water into 166.7g of silica sol with the solid content of 23.75wt.% for ball milling and mixing, wherein the ball milling and mixing time is 6 hours, and the rotating speed of ball milling and mixing is 300 revolutions per minute; drying in a 100 ℃ oven for 12 hours, crushing the dried mixture by using a pulverizer with the speed of 2 ten thousand revolutions per minute, and sieving by using a 3000-mesh sieve to obtain precursor powder; wherein Y is 2 O 3 And SiO 2 The molar ratio of the mixed slurry is 1:2.2, the solid content of the mixed slurry is 37.8 weight percent, and the nanometer Y is the nanometer Y 2 O 3 The purity of the powder is 99.99%, the grain diameter is 5 nm-50 nm, and the silica sol contains SiO 2 Aqueous solutions of nanoparticles, siO 2 Is amorphous SiO 2 The pH value of the silica sol is 2-3, and SiO in the silica sol 2 The particle diameter of the nano particles is 1 nm-5 nm.
S2, carrying out spark plasma sintering on the precursor powder obtained in the step S1 under the conditions of vacuum and no mechanical pressure, wherein the heating rate is 100 ℃/min, the reaction temperature is 1500 ℃, the heat preservation time is 5min, and finally naturally cooling to room temperature to obtain the product powder, namely the high-purity stable-phase gamma-yttrium disilicate ceramic powder.
XRD, SEM and EDS characterization is carried out on the product powder, and the phase composition and the microscopic morphology are respectively shown in figures 1 to 3. As can be seen from FIGS. 1 to 3, the gamma-Y prepared in this example 2 Si 2 O 7 The powder is almost pure phase, the purity is up to 98.7%, the microstructure is fused grains, partial agglomeration exists, the corresponding EDS result shows that the main components of the obtained particles are Y, si and O (wherein the element C is generally influenced by the substrate conductive adhesive), the corresponding atomic percentage is Y to Si to O=17.82 to 17.43 to 64.75, and the obtained particles are relatively close to the theoretical value (Y to Si to O=18.18 to 18.18 to 63.64), and the purity of the obtained product is further proved to be relatively high.
Comparative example 1
gamma-Y of this comparative example 2 Si 2 O 7 The preparation method of the powder is substantially the same as in example 1, except that:
in step S1, siO employed 2 The reaction raw material is alpha-SiO 2 Powder, unlike the silica sol of example 1, siO 2 Is amorphous SiO 2 。
gamma-Y prepared in this comparative example 2 Si 2 O 7 The phase composition of the powder is X2-Y 2 SiO 5 、β-Y 2 Si 2 O 7 And gamma-Y 2 Si 2 O 7 The mass percentages are 26.0%,8.1% and 65.9%, respectively. It can be seen that this comparative example product was of lower purity than example 1. This is due to alpha-SiO 2 The powder has an anisotropic crystal structure and Y 2 O 3 SiO with amorphous structure less contact than isotropy when reacting 2 Sufficient, additionally due to alpha-SiO 2 The powder raw materials are easy to settle when being dissolved in a water ball mill, unlike silica sol which is a uniformly dispersed suspension, the powder raw materials are not uniform in mixing under the condition of the same time of ball milling, and therefore the purity of the obtained product is not high.
Comparative example 2
gamma-Y of this comparative example 2 Si 2 O 7 The preparation method of the powder is substantially the same as in example 1, except that:
in step S1, nanoscale Y 2 O 3 SiO in powder and silica sol 2 The molar ratio of (2) was 1:2, which is different from the molar ratio of 1:2.2 of example 1.
gamma-Y prepared in this comparative example 2 Si 2 O 7 The phase composition of the powder is X2-Y 2 SiO 5 And gamma-Y 2 Si 2 O 7 The mass percentages of the two are 25.6% and 74.4% respectively. It can be seen that this comparative example product was of lower purity than example 1. This is due to gamma-Y 2 Si 2 O 7 The product is worked up, Y 2 O 3 With SiO 2 First, Y is generated in a molar ratio of 1:1 2 SiO 5 The obtained Y 2 SiO 5 And then doubling the molar ratio of SiO 2 Reacting to obtain the corresponding Y 2 Si 2 O 7 While in reality SiO 2 The powder can be decomposed partially in the high-temperature sintering process, when the molar ratio is strictly according to the reaction equation (1:2) SiO which actually participates in the reaction when the reaction raw material is supplied 2 In insufficient amounts, thereby resulting in a product with a certain amount of X2-Y 2 SiO 5 。
Comparative example 3
gamma-Y of this comparative example 2 Si 2 O 7 The preparation method of the powder is substantially the same as in example 1, except that:
in the step S2, the spark plasma sintering equipment is not adopted for sintering, but a traditional normal pressure sintering furnace is adopted, the heating rate is 5 ℃/min, the sintering temperature is 1500 ℃, and the heat preservation time is 120min.
gamma-Y prepared in this comparative example 2 Si 2 O 7 The phase composition of the powder is X2-Y 2 SiO 5 、γ-Y 2 Si 2 O 7 And Y 4.67 (SiO 4 ) 3 The mass percentages of O are 76.6%, 17.3% and 6.1%, respectively. It can be seen that this comparative example product was significantly less pure than example 1. The method is characterized in that the traditional normal pressure sintering furnace does not generate discharge among particles in the sintering process to realize local pre-melting, and the atomic diffusion rate is not as fast as the plasma discharge sintering rate under the same sintering temperature condition, so that the main phase in the product is X2-Y 2 SiO 5 。
Example 2
The preparation method of the high-purity stable phase gamma-yttrium disilicate ceramic powder comprises the following steps:
s1, 67.8g of nanoscale Y 2 O 3 Adding 50g of deionized water into 166.7g of silica sol with the solid content of 23.75wt.% for ball milling and mixing, wherein the ball milling and mixing time is 4 hours, and the ball milling and mixing rotating speed is 300 revolutions per minute to obtain mixed slurry; drying in a baking oven at 120 ℃ for 12 hours, crushing the dried mixture by using a pulverizer at 2 ten thousand revolutions per minute, and sieving by using a 5000-mesh sieve to obtain precursor powder; wherein Y is 2 O 3 And SiO 2 The molar ratio of the mixed slurry is 1:2.2, the solid content of the mixed slurry is 37.8 weight percent, and the nanometer Y is the nanometer Y 2 O 3 The purity of the powder is 99.99%, the grain diameter is 5 nm-50 nm, and the silica sol contains SiO 2 Aqueous solutions of nanoparticles, siO 2 Is amorphous SiO 2 The pH value of the silica sol is 2-3, and SiO 2 The particle diameter of the nano particles is 1 nm-5 nm.
S2, performing spark plasma sintering on the precursor powder obtained in the step S1 under the conditions of no mechanical pressure and nitrogen protection atmosphere (normal pressure), wherein the heating rate is 200 ℃/min, the reaction temperature is 1500 ℃, the heat preservation time is 5min, and finally naturally cooling to room temperature to obtain the product powder, namely the high-purity stable-phase gamma-yttrium disilicate ceramic powder. The gamma-Y prepared in this example was detected 2 Si 2 O 7 The purity of the ceramic powder was 97.0%.
The above description is only of the preferred embodiment of the present invention, and is not intended to limit the present invention in any way. While the invention has been described in terms of preferred embodiments, it is not intended to be limiting. Any person skilled in the art can make many possible variations and modifications to the technical solution of the present invention or equivalent embodiments using the method and technical solution disclosed above without departing from the spirit and technical solution of the present invention. Therefore, any simple modification, equivalent substitution, equivalent variation and modification of the above embodiments according to the technical substance of the present invention, which do not depart from the technical solution of the present invention, still fall within the scope of the technical solution of the present invention.
Claims (7)
1. The preparation method of the high-purity stable phase gamma-yttrium disilicate ceramic powder is characterized by comprising the following steps:
s1, nanometer Y 2 O 3 Adding the powder and the silica sol into water, ball-milling and mixing to obtain mixed slurry, drying, crushing and sieving to obtain precursor powder; wherein the silica sol contains SiO 2 Aqueous solutions of nanoparticles, siO 2 Is amorphous SiO 2 The nanometer level Y 2 O 3 Powder and SiO in the silica sol 2 The mol ratio of (2) is 1:2.1-2.3;
s2, performing spark plasma sintering on the obtained precursor powder under the conditions of protective atmosphere or vacuum or no mechanical pressure, and naturally cooling to obtain high-purity stable-phase gamma-yttrium disilicate ceramic powder, wherein the purity of the gamma-yttrium disilicate is more than 95%;
in step S1, the nanoscale Y 2 O 3 The purity of the powder is more than or equal to 99.99 percent, and the grain diameter is 5nm to 50nm; the solid content of the silica sol is 20wt.% to 40wt.%, the pH value is 2 to 3, and the SiO in the silica sol 2 The particle diameter of the nano particles is 1 nm-10 nm;
in the step S1, the ball milling and mixing time is 2-8 hours, and the rotating speed of the ball milling and mixing is 200-500 rpm; the drying temperature is 60-150 ℃, and the drying time is 8-24 hours; the rotational speed adopted by the crushing is 2-3 ten thousand rpm, and the mesh number of the sieving is 500-5000 meshes;
in the step S2, the heating rate of the spark plasma sintering is 50 ℃/min-300 ℃/min, the sintering temperature is 1450-1600 ℃, and the heat preservation time is 1-10 min.
2. The method for preparing high purity stable phase gamma-yttrium disilicate ceramic powder according to claim 1, wherein in step S1, the nanoscale Y 2 O 3 Powder and SiO in the silica sol 2 The molar ratio of the mixed slurry is 1:2.15-2.25, and the solid content of the mixed slurry is 30-60 wt.%.
3. The method for preparing high purity stable phase gamma-yttrium disilicate ceramic powder according to claim 1, wherein in step S1, the nanoscale Y 2 O 3 The particle size of the powder is 5 nm-10 nm; siO in the silica sol 2 The particle diameter of the nano particles is 1 nm-3 nm.
4. The method for preparing high-purity stable phase gamma-yttrium disilicate ceramic powder according to any one of claims 1 to 3, wherein in step S1, the time of the ball-milling mixing is 4h to 6h, and the rotational speed of the ball-milling mixing is 300 rpm to 400 rpm; the drying temperature is 80-100 ℃, and the drying time is 12-16 h; the mesh number of the sieve is 1000-2000 meshes.
5. The method for preparing high-purity stable phase gamma-yttrium disilicate ceramic powder according to any one of claims 1 to 3, wherein in the step S2, the temperature rising rate of the spark plasma sintering is 100 ℃/min to 150 ℃/min, the sintering temperature is 1500 ℃ to 1560 ℃ and the heat preservation time is 3min to 6min.
6. The method for preparing high-purity stable phase gamma-yttrium disilicate ceramic powder according to any of claims 1 to 3, wherein in the step S2, the protective atmosphere is one or more of nitrogen, helium and argon.
7. A highly pure stable phase gamma-yttrium disilicate ceramic powder prepared by the method of any of claims 1 to 6.
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| CN114436656A (en) * | 2022-01-29 | 2022-05-06 | 北京工业大学 | High-entropy silicate ceramic with low thermal conductivity and high thermal stability and preparation method and application thereof |
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| CN101391796A (en) * | 2008-10-29 | 2009-03-25 | 陕西科技大学 | Method for preparing yttrium silicate nano powder |
| JP2010208901A (en) * | 2009-03-11 | 2010-09-24 | Nippon Soken Inc | Alumina sintered compact, method for producing the same, and spark plug obtained by using the same |
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