CN109665846A - A method of crystalline ceramics is prepared using commercially available calcirm-fluoride powder as material vacuum hot pressed sintering - Google Patents
A method of crystalline ceramics is prepared using commercially available calcirm-fluoride powder as material vacuum hot pressed sintering Download PDFInfo
- Publication number
- CN109665846A CN109665846A CN201811544758.6A CN201811544758A CN109665846A CN 109665846 A CN109665846 A CN 109665846A CN 201811544758 A CN201811544758 A CN 201811544758A CN 109665846 A CN109665846 A CN 109665846A
- Authority
- CN
- China
- Prior art keywords
- calcirm
- powder
- fluoride
- crystalline ceramics
- commercially available
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/553—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on fluorides
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
- C04B35/645—Pressure sintering
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6562—Heating rate
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/658—Atmosphere during thermal treatment
- C04B2235/6581—Total pressure below 1 atmosphere, e.g. vacuum
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
- C04B2235/9646—Optical properties
- C04B2235/9653—Translucent or transparent ceramics other than alumina
Abstract
The invention discloses a kind of methods for preparing crystalline ceramics as material vacuum hot pressed sintering using commercially available calcirm-fluoride powder, and steps are as follows: 1) using commercially available calcirm-fluoride powder as raw material, adding the sodium fluoride powder of set amount, mix；2) graphite jig is selected, mixed-powder is fitted into mold, is separated mold and powder with graphite paper；3) graphite jig filled is put into vacuum hotpressing stove and is sintered；4) after being sintered, ceramics are polished to get calcirm-fluoride crystalline ceramics is arrived.Compared with existing calcirm-fluoride crystalline ceramics preparation method, present invention has an advantage that the process of no chemical method synthetic powder reduces the discharge of chemical waste, and shortens manufacturing cycle directly using commercially available calcirm-fluoride powder as raw material；The present invention prepares calcirm-fluoride crystalline ceramics using vacuum hot pressing sintering technique, and required equipment price is low, easier to operate.Present invention optimizes existing calcirm-fluoride crystalline ceramics preparation processes, reduce preparation cost.The calcirm-fluoride crystalline ceramics that the present invention prepares has good transparency.
Description
Technical field
The present invention relates to fluoride crystalline ceramics preparation field, specially one kind is led to using commercially available calcirm-fluoride powder as raw material
Cross the method that vacuum heating-press sintering prepares crystalline ceramics.
Background technique
Calcirm-fluoride (CaF2) it is the very excellent optical material of a kind of comprehensive performance, there is transmitance height, transmission peak wavelength model
Width and the low equal excellent properties of phonon energy are enclosed, are widely used in the fields such as industry and scientific research.Currently, CaF2Optical material master
It will be based on monocrystalline and glass-ceramic.Crystalline ceramics not only has the resistance to height of ceramics inherently as a kind of novel optical material
The advantages that warm, corrosion-resistant and high-intensitive, also have with optical property as glass phase, compared with monocrystalline, preparation process is simpler
It is single.In recent years, with the fast development of crystalline ceramics theory and technology of preparing, calcirm-fluoride crystalline ceramics is prepared by researchers
Attention.Currently, being primarily present two approach prepares calcirm-fluoride crystalline ceramics: first is that in the high temperature environment to CaF2Crystal applies
Pressure makes it occur being changed from monocrystalline to polycrystalline, obtains calcirm-fluoride crystalline ceramics；Another approach is with calcirm-fluoride powder for original
Material, prepares calcirm-fluoride crystalline ceramics by ceramic sintering technology.
In the technique for preparing calcirm-fluoride crystalline ceramics as raw material using powder, because commercially available calcirm-fluoride powder sintering activity is opposite
Lower, powder raw material used is mainly the calcirm-fluoride powder synthesized by chemical method.Currently, being original with commercially available calcirm-fluoride powder
Material is prepared in the research of crystalline ceramics, mainly using discharge plasma sintering technology (SPS) (referring to document F Nakamura,
T Kato, G Okada, et al. Scintillation and dosimeter properties of CaF2
transparent ceramics doped with Nd3+ produced by SPS, J. Eur. Ceram. Soc. 37
(2017) 4919-4924).The method required temperature is high, and carburization phenomena is more serious, and calcium fluoride ceramic transparency is low and sample holds
Easy blackening.There is researcher by a kind of improved discharge plasma sintering process, prepares the good calcirm-fluoride pottery of transparency
Porcelain is (referring to document P Wang, M Yang, S Zhang, et al. Suppression of carbon
contamination in SPSed CaF2 transparent ceramics by Mo foil, J. Eur. Ceram.
Soc. 37 (2017) 4103-4107), but the crystalline ceramics that the method is prepared is easy to crack, required sintering temperature and pressure
Also higher.Hot pressing and sintering technique can be heated and be pressurizeed to powder raw material simultaneously, be that prepare calcirm-fluoride using synthetic powder as raw material saturating
The main sintering method of bright ceramics.Compared with discharge plasma sintering technology, equipment needed for vacuum hot pressing sintering technique is simple,
Strong operability.Recently, researcher attempts to prepare calcirm-fluoride by vacuum heating-press sintering using commercially available calcirm-fluoride powder as raw material
Ceramics, because commercially available calcirm-fluoride powder sintering activity is low, the calcium fluoride ceramic prepared it is completely opaque (referring to document W Li,
H Huang, B Mei, et al. Comparison of commercial and synthesized CaF2 powders
43 (2017) 10403-10409 of for preparing transparent ceramics, Ceram. Int.).
Therefore, a kind of method that crystalline ceramics is prepared as material vacuum hot pressed sintering using commercially available calcirm-fluoride powder is developed, it is excellent
Change existing calcirm-fluoride crystalline ceramics preparation process, has great importance.
Summary of the invention
In order to solve above-mentioned the deficiencies in the prior art, it is original that the present invention provides one kind with commercially available calcirm-fluoride powder
Material, the method that calcirm-fluoride crystalline ceramics is prepared by vacuum hot pressing sintering technique.
The object of the present invention is achieved like this:
A method of crystalline ceramics being prepared by material vacuum hot pressed sintering of commercially available calcirm-fluoride powder, key step includes powder
The preparation of raw material and the sintering of crystalline ceramics, specific steps include:
1) preparation of powder raw material: weighing the commercially available calcirm-fluoride powder of setting quality, set amount sodium fluoride powder is added, with anhydrous
Ethyl alcohol is medium, and the two is mixed, and is dried for standby；
2) powder raw material fills sample: selecting graphite jig, the mixed-powder after drying in step 1) is fitted into mold, and use graphite
Paper separates mold and powder raw material；
3) sintering of crystalline ceramics: the graphite jig in step 2 is put into vacuum hotpressing stove and is sintered；
4) processing of crystalline ceramics: after sintering, the ceramics in step 3) are taken out, after being roughly ground using sand paper, in polishing machine
On ceramics sample is processed by shot blasting, obtain calcirm-fluoride crystalline ceramics.
Calcirm-fluoride powder used is commercially available, purity >=99% in the step 1)；
Added sodium fluoride powder is commercially available, purity >=99%, diameter of particle≤20 μm in the step 1)；
In the step 1) calcirm-fluoride and sodium fluoride mixed-powder, the content of sodium fluoride is 0.5mol%-5 mol%；
Sintering method is vacuum heating-press sintering in the step 3), and vacuum degree≤10Pa, sintering temperature is at 750 DEG C -900 DEG C；
Soaking time is 3h-10h in the step 3), and for heating rate in 5 DEG C/min-20 DEG C/min, pressure is 20 MPa-
50MPa。
Positive beneficial effect: directly using commercially available calcirm-fluoride powder as raw material, the process of no synthetic powder raw material subtracts the present invention
Lack the discharge of chemical waste in crystalline ceramics preparation process, and shortens manufacturing cycle；In addition, the present invention uses Vacuum Heat
Pressure sintering technology prepares crystalline ceramics, and required equipment price is low, easier to operate；Present invention optimizes the preparations of calcirm-fluoride crystalline ceramics
Technique reduces preparation cost；The calcirm-fluoride crystalline ceramics that the present invention prepares has good transparency.
Detailed description of the invention
Fig. 1 is that commercially available calcirm-fluoride powder used in the present invention amplifies 500 times of picture schematic diagrames；
Fig. 2 is that commercially available calcirm-fluoride powder used in the present invention amplifies 10000 times of picture schematic diagrames；
Fig. 3 is that sodium fluoride powder used in the present invention amplifies 3000 times of picture schematic diagrames；
Fig. 4 is the calcirm-fluoride crystalline ceramics picture prepared at 800 DEG C.
Specific embodiment
In order to better understand the present invention, the present invention with reference to the accompanying drawing, is described in detail preferred embodiment.But
The present invention is not limited in following examples.On the contrary, provide these examples be in order to explain and illustrate basic principle of the invention and
Practical application, to enable others skilled in the art to understand the present invention and make specific expected modification.If without spy
Do not mentionlet alone bright, the various raw materials that use and other consumptive materials can be commercially available by market in the present invention.
Embodiment 1
1) preparation of powder raw material: weighing the commercially available calcirm-fluoride powder of 5g, adds sodium fluoride powder, makes the content of sodium fluoride
5mol%, calcirm-fluoride and sodium fluoride powder mix well in alcohol, and then mixed-powder is put into baking oven and is dried；
2) powder raw material fills sample: selecting internal diameter is the graphite jig of 16 mm, in a mold one layer of graphite paper of pad, weighs 2g step
The rapid mixed-powder 1) obtained is fitted into mold, is separated mold and mixed-powder with graphite paper；
3) sintering of crystalline ceramics: the graphite jig filled is put into vacuum hotpressing stove, is evacuated to better than 10Pa, with 5
DEG C/rate of min is warming up to 800 DEG C, then apply pressure 30MPa, keeps the temperature 3h；
4) processing of crystalline ceramics: after sintering, ceramics sample is taken out, after first being roughly ground with sand paper, then to sample on polishing machine
Product are processed by shot blasting to get to the calcirm-fluoride crystalline ceramics being sintered at a temperature of 800 DEG C.
If Fig. 1 is commercially available calcirm-fluoride powder picture used in the present invention (500 times of amplification), powder raw material is agglomerated into partial size and is
Tens microns of bulky grain.Fig. 2 is commercially available calcirm-fluoride powder picture used in the present invention (10000 times of amplification), it can be seen that Fig. 1
In bulky grain be by reuniting having a size of tens nanometers of powder.Fig. 3 is that sodium fluoride powder picture used in the present invention (is put
It is 3000 times big), partial size is not more than 20 μm.Fig. 4 is the calcirm-fluoride crystalline ceramics picture prepared at 800 DEG C, and ceramics have very
Good transparency, can tell the pattern under ceramics.
Embodiment 2
1) preparation of powder raw material: weighing the commercially available calcirm-fluoride powder of 5g, adds sodium fluoride powder, makes the content of sodium fluoride
0.5mol%, calcirm-fluoride and sodium fluoride powder mix well in alcohol, and then mixed-powder is put into baking oven and is dried；
2) powder raw material fills sample: selecting internal diameter is the graphite jig of 16 mm, in a mold one layer of graphite paper of pad, weighs 2g step
The rapid mixed-powder 1) obtained is fitted into mold, is separated mold and mixed-powder with graphite paper；
3) sintering of crystalline ceramics: the graphite jig filled is put into vacuum hotpressing stove, is evacuated to better than 10Pa, with 20
DEG C/rate of min is warming up to 900 DEG C, then apply 50 MPa of pressure, keeps the temperature 10h；
4) processing of crystalline ceramics: after sintering, ceramics sample is taken out, after first being roughly ground with sand paper, then to sample on polishing machine
Product are processed by shot blasting to get to the calcirm-fluoride crystalline ceramics being sintered at a temperature of 900 DEG C.
Embodiment 3
1) preparation of powder raw material: weighing the commercially available calcirm-fluoride powder of 5g, adds sodium fluoride powder, makes the content of sodium fluoride
5mol%, calcirm-fluoride and sodium fluoride powder mix well in alcohol, and then mixed-powder is put into baking oven and is dried；
2) powder raw material fills sample: selecting internal diameter is the graphite jig of 16 mm, in a mold one layer of graphite paper of pad, weighs 2g step
The rapid mixed-powder 1) obtained is fitted into mold, is separated mold and mixed-powder with graphite paper；
3) sintering of crystalline ceramics: the graphite jig filled is put into vacuum hotpressing stove, is evacuated to better than 10Pa, with 10
DEG C/rate of min is warming up to 750 DEG C, then apply 50 MPa of pressure, keeps the temperature 10h；
4) processing of crystalline ceramics: after sintering, ceramics sample is taken out, after first being roughly ground with sand paper, then to sample on polishing machine
Product are processed by shot blasting to get to the calcirm-fluoride crystalline ceramics being sintered at a temperature of 750 DEG C.
Embodiment 4
1) preparation of powder raw material: weighing the commercially available calcirm-fluoride powder of 5g, adds sodium fluoride powder, makes the content of sodium fluoride
3mol%, calcirm-fluoride and sodium fluoride powder mix well in alcohol, and then mixed-powder is put into baking oven and is dried；
2) powder raw material fills sample: selecting internal diameter is the graphite jig of 16 mm, in a mold one layer of graphite paper of pad, weighs 2g step
The rapid mixed-powder 1) obtained is fitted into mold, is separated mold and mixed-powder with graphite paper；
3) sintering of crystalline ceramics: the graphite jig filled is put into vacuum hotpressing stove, is evacuated to better than 10Pa, with 10
DEG C/rate of min is warming up to 850 DEG C, then apply pressure 20MPa, keeps the temperature 5h；
4) processing of crystalline ceramics: after sintering, ceramics sample is taken out, after first being roughly ground with sand paper, then to sample on polishing machine
Product are processed by shot blasting to get to the calcirm-fluoride crystalline ceramics being sintered at a temperature of 850 DEG C.
For the present invention directly using commercially available calcirm-fluoride powder as raw material, the process of no synthetic powder raw material reduces crystalline ceramics
The discharge of chemical waste in preparation process, and shorten manufacturing cycle；In addition, the present invention uses vacuum hot pressing sintering technique system
Standby crystalline ceramics, required equipment price is low, easier to operate；Present invention optimizes calcirm-fluoride crystalline ceramics preparation processes, reduce
Preparation cost；The calcirm-fluoride crystalline ceramics that the present invention prepares has good transparency.
It should finally be noted the above description is only a preferred embodiment of the present invention, it is served only for technical solution of the present invention
It is described in more detail.Conceive according to the present invention for those skilled in the art the nonessential improvement of make several and
Adjustment, all belongs to the scope of protection of the present invention.
Claims (6)
1. a kind of method for preparing crystalline ceramics as material vacuum hot pressed sintering using commercially available calcirm-fluoride powder, it is characterised in that: with
Commercially available calcirm-fluoride powder is raw material, adds the sodium fluoride powder of set amount, prepares the transparent pottery of calcirm-fluoride by vacuum heating-press sintering
Porcelain, key step include the preparation of powder raw material and the sintering of crystalline ceramics, and specific steps include:
1) the commercially available calcirm-fluoride powder of setting quality, addition setting sodium fluoride powder, with anhydrous second the preparation of powder raw material: are weighed
Alcohol is medium, and the two is mixed, and is dried for standby；
2) powder raw material fills sample: selecting graphite jig, the mixed-powder after drying in step 1) is fitted into mold, and use graphite
Paper separates mold and powder raw material；
3) sintering of crystalline ceramics: the graphite jig in step 2 is put into vacuum hotpressing stove and is sintered；
4) processing of crystalline ceramics: after sintering, the ceramics in step 3) are taken out, after being roughly ground using sand paper, in polishing machine
On ceramics sample is processed by shot blasting, obtain calcirm-fluoride crystalline ceramics.
2. according to claim 1 a kind of crystalline ceramics is prepared using commercially available calcirm-fluoride powder as material vacuum hot pressed sintering
Method, it is characterised in that: calcirm-fluoride powder used is commercially available, purity >=99% in the step 1).
3. according to claim 1 a kind of crystalline ceramics is prepared using commercially available calcirm-fluoride powder as material vacuum hot pressed sintering
Method, it is characterised in that: added sodium fluoride powder is commercially available, purity >=99%, diameter of particle≤20 in the step 1)
μm。
4. according to claim 1 a kind of crystalline ceramics is prepared using commercially available calcirm-fluoride powder as material vacuum hot pressed sintering
Method, it is characterised in that: in the step 1) calcirm-fluoride and sodium fluoride mixed-powder, the content of sodium fluoride is 0.5mol%-5
mol%。
5. according to claim 1 a kind of crystalline ceramics is prepared using commercially available calcirm-fluoride powder as material vacuum hot pressed sintering
Method, it is characterised in that: sintering method is vacuum heating-press sintering in the step 3), and vacuum degree≤10Pa, sintering temperature exists
750℃-900℃。
6. according to claim 1 a kind of crystalline ceramics is prepared using commercially available calcirm-fluoride powder as material vacuum hot pressed sintering
Method, it is characterised in that: soaking time is 3h-10h in the step 3), and heating rate is in 5 DEG C/min-20 DEG C/min, pressure
Power is 20 MPa-50MPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811544758.6A CN109665846A (en) | 2018-12-17 | 2018-12-17 | A method of crystalline ceramics is prepared using commercially available calcirm-fluoride powder as material vacuum hot pressed sintering |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811544758.6A CN109665846A (en) | 2018-12-17 | 2018-12-17 | A method of crystalline ceramics is prepared using commercially available calcirm-fluoride powder as material vacuum hot pressed sintering |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109665846A true CN109665846A (en) | 2019-04-23 |
Family
ID=66143951
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811544758.6A Pending CN109665846A (en) | 2018-12-17 | 2018-12-17 | A method of crystalline ceramics is prepared using commercially available calcirm-fluoride powder as material vacuum hot pressed sintering |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109665846A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116529203A (en) * | 2020-12-28 | 2023-08-01 | 株式会社 尼康 | Sintered calcium fluoride, method for producing sintered calcium fluoride particles, optical element, optical system, interchangeable lens, and optical device |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05294724A (en) * | 1992-04-10 | 1993-11-09 | Kurosaki Refract Co Ltd | Production of polycrystalline transparent yag ceramic for solid laser |
| CN102126857A (en) * | 2011-01-31 | 2011-07-20 | 武汉理工大学 | Method for preparing transparent calcium fluoride ceramic |
| CN107200582A (en) * | 2017-06-08 | 2017-09-26 | 信阳师范学院 | A kind of method that polycrystalline transparent ceramic is prepared by raw material of Natural Fluorite mineral |
-
2018
- 2018-12-17 CN CN201811544758.6A patent/CN109665846A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05294724A (en) * | 1992-04-10 | 1993-11-09 | Kurosaki Refract Co Ltd | Production of polycrystalline transparent yag ceramic for solid laser |
| CN102126857A (en) * | 2011-01-31 | 2011-07-20 | 武汉理工大学 | Method for preparing transparent calcium fluoride ceramic |
| CN107200582A (en) * | 2017-06-08 | 2017-09-26 | 信阳师范学院 | A kind of method that polycrystalline transparent ceramic is prepared by raw material of Natural Fluorite mineral |
Non-Patent Citations (1)
| Title |
|---|
| 劳动人事部《职业卫生与安全百科全书》译审委员会: "《职业卫生与安全百科全书 上下》", 30 September 1987, 中国大百科全书出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116529203A (en) * | 2020-12-28 | 2023-08-01 | 株式会社 尼康 | Sintered calcium fluoride, method for producing sintered calcium fluoride particles, optical element, optical system, interchangeable lens, and optical device |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106478105B (en) | A kind of method that multistep reaction sintering process prepares the thyrite of low residual silicon | |
| CN103396121B (en) | Novel transparent glitter ceramic with garnet structure and preparation method thereof | |
| CN102020470B (en) | Preparation method of transparent yttria ceramics with high optical quality | |
| CN101817683B (en) | Method for preparing MgAlON transparent ceramic in pressureless sintering way | |
| CN103553629B (en) | Method for preparing aluminum oxynitride transparent ceramic through gel casting | |
| CN102126857B (en) | Method for preparing transparent calcium fluoride ceramic | |
| CN101935208B (en) | Rare earth aluminate single-phase or complex-phase nanocrystalline transparent ceramic material and preparation method thereof | |
| CN102311258B (en) | Active ion controlled doping yttrium aluminum garnet base laser transparent ceramic material and preparation method thereof | |
| JP2016041648A (en) | Method for manufacturing gadolinium oxysulfide ceramic scintillator | |
| CN112299861B (en) | AlON transparent ceramic pseudo-sintering agent and application thereof, and preparation method of transparent ceramic | |
| CN103011827A (en) | Preparation method of zirconium diboride ceramic with in-situ-introduced boron as additive | |
| CN106966700A (en) | A kind of short route preparation technology of tin indium oxide sintered body | |
| CN103833403A (en) | Preparation method of silicon carbide whisker toughened boron carbide (B4C) ceramic composite material and product thereof | |
| CN108546109B (en) | Preparation method of large-size AZO magnetron sputtering target with controllable oxygen vacancy | |
| CN110835781B (en) | Blackening method of lithium niobate or lithium tantalate wafer | |
| CN107857261A (en) | A kind of preparation method of nuclear graphite materials | |
| CN101734918A (en) | Compact 10 B boron carbide-rich ceramics and preparation thereof | |
| Duan et al. | Fabrication of transparent Tb3Al5O12 ceramics by hot isostatic pressing sintering | |
| CN103482970B (en) | A kind of laser transparent ceramic and preparation method thereof | |
| CN109665846A (en) | A method of crystalline ceramics is prepared using commercially available calcirm-fluoride powder as material vacuum hot pressed sintering | |
| CN102786304A (en) | Preparation method for hot-pressed boron carbide ceramic | |
| CN103755353B (en) | A kind of fast low temperature preparation method of Y-α-SiAlON crystalline ceramics | |
| CN110282959A (en) | A kind of method of graphene Strengthening and Toughening aluminium oxide ceramics | |
| CN109574671A (en) | It is a kind of using sodium fluoride as the preparation method of the fluorite mineral polycrystalline transparent ceramic of auxiliary agent | |
| CN110759733B (en) | Y0.5Dy0.5Ta0.5Nb0.5O4Tantalum ceramic material and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190423 |
|
| RJ01 | Rejection of invention patent application after publication |