CN101830694A - High-purity stannic oxide electrode ceramic material and preparation method thereof - Google Patents
High-purity stannic oxide electrode ceramic material and preparation method thereof Download PDFInfo
- Publication number
- CN101830694A CN101830694A CN 201010171545 CN201010171545A CN101830694A CN 101830694 A CN101830694 A CN 101830694A CN 201010171545 CN201010171545 CN 201010171545 CN 201010171545 A CN201010171545 A CN 201010171545A CN 101830694 A CN101830694 A CN 101830694A
- Authority
- CN
- China
- Prior art keywords
- weight part
- powder
- weight
- ceramic material
- sno
- 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.)
- Granted
Links
Abstract
The invention discloses a stannic oxide electrode ceramic material and a preparation method thereof. The stannic oxide electrode ceramic material is prepared from high-purity SnO2 powder, high-purity auxiliary materials of Sb2O3, ZnO and Pr6O11 and a water solution of sodium silicate as an active agent according to specified ratio by using a specified processing technique. The service temperature of the stannic oxide electrode ceramic material is 1,500-1,550DEG C. In addition, the copper content of the stannic oxide electrode ceramic material, which is determined by using an atom absorbing method, is less than 20ppm. The invention is applicable for producing phosphate laser glass.
Description
Technical field
The present invention relates to high-purity stannic oxide electrode ceramic material and preparation method thereof.This material is used for the phosphoric acid salt laser glass, also can be used for plumbous oxide content less than 66% various artistic glass.
Background technology
The open CN85100034A of Chinese patent relates to the electrode of electromagnetic flowmeter material that is made of tin dioxide conductive ceramics, belongs to pottery; The prescription of this electrode materials is: SnO
2Be 100%; CuO is 0～5%; Sb
2O
3Be 0.1～10%; ZnO is 0.4～2%; PbO is 0.007%; Fe
2O
3Be 0.05%.This pottery adopts ordinary ceramic process, burns till under 1300～1360 ℃ under oxidizing atmosphere, and its characteristic is the erosion of the various concentration strong acid of ability, and normal temperature conducts electricity very well.
Chinese patent application 200710048050.7 (CN101182096A) relates to the preparation method of the stannic oxide electrode that a kind of glass electric furnace uses, and may further comprise the steps: (1) is with tin tetrachloride SnCl
4With metal chloride be raw material, adopt chemical coprecipitation to make precursor, 550 ℃-650 ℃ calcinings 1-2 hour down, the tindioxide superfine powder of 1%～3% metal oxide that evenly mixed; (2),, promptly obtain density＞6.5g/cm 1250～1400 ℃ of following sintering 3～8 hours by waiting static pressure 200MPa moulding
3The high compactness stannic oxide electrode.
Chinese patent application 200810237418.9 (CN101439966A) discloses the preparation method of stannic oxide electrode ceramic material, comprises the steps: 1) batching: the quality by sintering aid is SnO
2The 0.5-1.0% of powder quality chooses sintering aid and SnO
2Powder, wherein, sintering aid is MnO
2Powder and CuO powder, MnO
2Powder, CuO powder shared mass percent in sintering aid is: MnO
2Powder 5-95%, CuO powder 5-95%; Press Sb
2O
3The quality of powder is SnO
2The 0.1-1.0% of powder quality chooses Sb
2O
3Powder, standby; 2) granulation: with SnO
2Powder, CuO powder, MnO
2Powder, Sb
2O
3Powder, organic solvent and batch mixing ball are put into ball grinder, mix in planetary ball mill; The slurry that mixes is poured in the container, put into baking oven and carry out low-temperature bake and finish, grind, cross the opening sieve then, obtain mixed powder until organic solvent volatilization; 3) cold isostatic compaction: mixed powder is put into mould,, get base substrate by the cold isostatic press moulding; 4) pressureless sintering: base substrate is put into the sintering oven sintering, get stannic oxide electrode ceramic material.
Chinese patent application 200810237419.3 (CN101439967A) discloses a kind of preparation method of high compactness stannic oxide ceramic, and it comprises the steps: 1) batching: the quality by sintering aid is SnO
20.5～5.0% of powder quality is chosen sintering aid and SnO
2Powder, wherein, sintering aid is MnO
2Powder and CuO powder, MnO
2Powder, CuO powder shared mass percent in sintering aid is: MnO
2Powder 5～95%, CuO powder 5～95%; 2) ball mill mixing: with SnO
2Powder, CuO powder, MnO
2Powder, organic solvent and batch mixing ball are put into ball grinder, mix in planetary ball mill, get slurry; 3) oven dry: slurry is poured in the Glass Containers, put into baking oven and carry out low-temperature bake and finish, grind the back and cross the opening sieve, obtain mixed powder until solvent evaporates; 4) calm molded: mixed powder is carried out die forming, vacuumize after putting into plastic jacket, the vacuum state plastic jacket that mixed powder will be housed is again put into the cold isostatic press moulding, base substrate; 5) pressureless sintering: the base substrate of acquisition is put into the sintering oven sintering, obtains high compactness stannic oxide ceramic.
Tin oxide electrode in the disclosed technology generally adds copper or manganese.And neither adding copper, the present invention do not add manganese yet.The advantage of prior art is that price is relatively cheap, but has following shortcoming: 1, use temperature is lower; 2, normal temperature resistance is bigger; 3, easily make glass coloring; 4, be not suitable for laser glass.
Purpose of the present invention
The invention provides a kind of preparation method of novel stannic oxide electrode ceramic material, overcome the shortcoming of prior art, this method may further comprise the steps:
1) powder mixes: according to the ratio weighing of prescription, earlier water glass is dissolved in a certain amount of pure water, then (for example diameter is 8-12mm, preferred 9-11mm, more preferably 10mm) zirconium oxide balls adds in the ball milling, adds powder and additive mixing and ball milling then respectively; Ball mill can be with inorganic corundum matter ball grinder.Ball milling mixing time 2～30 hours.
2) drying: with mixed slurry in Electric heat oven more than 120 ℃ temperature baking detect moisture less than 0.3% by national standard more than 14 hours.
3) pulverize: the opening that the blended powder was ground below 30 orders sieves, and obtains uniform mixed powder.
4) cold isostatic compaction: in powder dress punching block if any gum cover, the pressure pressurize of 200～250MPa 3～10 minutes, press base substrate.
5) base substrate finishing: repair billet surface smooth.
6) do not have to press the neutral atmosphere sintering: base substrate is packed into makes high-purity stannic oxide electrode ceramic material of the present invention through 1450～1550 ℃ of insulations calcining in 3～20 hours in the sintering oven.
Technical solution of the present invention
Employed in the present invention raw material has: SnO
2Sb
2O
3ZnO; Pr
6O
11And sodium silicate aqueous solution.SnO
2, Sb
2O
3, ZnO and Pr
6O
11Four kinds of raw materials preferably all are powder (fine particle) or coarse particles form.For pulverous raw material, its mean particle size is＜600 μ m preferred＜300 μ m, more preferably＜100 μ m, more more preferably＜50 μ m, most preferably 0.5-5 μ m; For the raw material of coarse particles shape, its mean particle size is between 600 μ m to 5000 μ m, preferably between 600 μ m to 2000 μ m, more preferably between 300 μ m to 1000 μ m, more more preferably between 100 μ m to 500 μ m.
" mean particle size " refers to expect equal granularity in the present invention, unless otherwise mentioned.
Sb in the present invention
2O
3, ZnO and Pr
6O
11As additive; Water glass is made promoting agent, generally is to use with the form of the aqueous solution.
Preferably, employed raw material is: SnO
2, purity 〉=99.5%; Sb
2O
3, purity 〉=99.5%; ZnO, purity 〉=99.5%; Pr
6O
11, purity 〉=99%; With degree Beaume be 52% sodium silicate aqueous solution.In the present invention, the special raw material that uses in an embodiment all requires to satisfy above requirement.
The relative weight ratio of raw material is in the present invention: 100 parts of SnO
2, 0.5～1.5 part of (preferred 0.7～1.3, more preferably 0.8～1.1) Sb
2O
3, 0.1～1.5 part of (preferred 0.3～1.3, more preferably 0.5～1.1) ZnO, 0.1～1.5 part of (preferred 0.2～1.1, more preferably 0.3～0.8) Pr
6O
11, the sodium silicate aqueous solution of 0.05～0.5 part (preferred 0.1～0.3, more preferably 0.15～0.25).Preferably, SnO wherein
2Purity 〉=99.5%; Sb
2O
3Purity 〉=99.5%; ZnO purity 〉=99.5%; Pr
6O
11Purity 〉=99%; With sodium silicate aqueous solution be that degree Beaume is the sodium silicate aqueous solution of 46～55% (preferred 50～52%) (being recorded by Beaum).
Generally in mechanical milling process, various additives (are Sb
2O
3, ZnO and Pr
6O
11) and SnO
2The part by weight of powder and abrading-ball is 1: 0.9～2.0, preferred 1: 1.0～1.5, more preferably 1: 1.1～1.3, add 25～40% pure water mixing and ball milling 2～30 hours (preferred 3～20 hours, more preferably 4～15 hours).
Water glass is dissolved in makes the sodium silicate aqueous solution that degree Beaume is 46～55% (preferred 50～52%) in the pure water, standby.
Most preferably, the tindioxide powder as raw material satisfies following technical indicator:
SnO
2〉=99.5%; Cu≤3PPM; Fe≤150PPM; Pb≤140PPM; Burn and lose≤0.025%; Whiteness 〉=84.5; Account for whole SnO
2The SnO of the ratio that the 98wt% of powder total amount is above
2Powder has＜5 microns granularity.
In first embodiment of the present invention, the preparation method of stannic oxide electrode ceramic material is provided, it comprises the steps:
1) ball milling processing:
According to following material rate weighing: the SnO of 100 weight parts
2Powder, the Sb of 0.5～1.5 weight part (preferred 0.6～1.3, more preferably 0.7～1.1)
2O
3, the ZnO of 0.1～1.5 weight part (preferred 0.6～1.3, more preferably 0.7～1.1), the Pr of 0.1～1.5 weight part (preferred 0.2～1.1, more preferably 0.3～0.8)
6O
11, Sb wherein
2O
3, ZnO and Pr
6O
11The weight summation be 1.0-3.0 weight part (preferred 1.5-2.5 weight part, more preferably 2.2 weight parts), the sodium silicate aqueous solution of 0.05～0.5 weight part (preferred 0.1～0.3, more preferably 0.15～0.25);
Mechanical milling process: above 0.1～1.0 weight part sodium silicate aqueous solution of having got ready is dissolved in or be blended in the water of 10-35 weight part (preferred 15-30 weight part) after join in the ball mill, then add SnO
2Powder and additive Sb
2O
3, ZnO and Pr
6O
11, add the water of 35～10 weight parts again, sealing mixing and ball milling 2～30 hours (preferred 3～20 hours, more preferably 4～15 hours);
2) drying;
3) pulverize;
4) cold isostatic compaction;
5) optional base substrate is repaired: repair billet surface smooth;
6) sintering.
In second embodiment based on first embodiment of the present invention, the preparation method of stannic oxide electrode ceramic material is provided, it comprises the steps:
1) ball milling processing:
According to following material rate weighing: the SnO of 100 weight parts
2Powder (mean particle size 5～0.5 μ m), the Sb of 0.5～1.5 weight part (preferred 0.6～1.3, more preferably 0.7～1.1)
2O
3(mean particle size 5～0.5 μ m), the ZnO (mean particle size 5～0.5 μ m) of 0.1～1.5 weight part (preferred 0.6～1.3, more preferably 0.7～1.1), the Pr of 0.1～1.5 weight part (preferred 0.2～1.1, more preferably 0.3～0.8)
6O
11(mean particle size 5～0.5 μ m), wherein Sb
2O
3, ZnO and Pr
6O
11The weight summation be 1.0-3.0 weight part (preferred 1.5-2.5 weight part, more preferably 2.2 weight parts), the sodium silicate aqueous solution of 0.05～1.0 weight part (preferred 0.1～0.5, more preferably 0.15～0.25);
Mechanical milling process: above 0.05～1.0 weight part sodium silicate aqueous solution of having got ready is dissolved in or be blended in the water of 10-35 weight part (for example 15 or 25 weight parts) after join in the ball mill, then 40～60 weight parts (for example 50 weight parts) (for example diameter is 8-12mm, preferred 10mm) (preferably, requiring various additives (is Sb in the zirconium oxide balls adding ball mill
2O
3, ZnO and Pr
6O
11) and SnO
2The part by weight of powder and abrading-ball is 1: 0.9～2.0 (preferred 1: 1.2～1.6)), adding accounts for SnO respectively then
2The SnO of 35～65wt% of the total consumption of powder (i.e. 100 weight parts) (preferred 40～60%, more preferably 50wt%)
2Powder, whole consumption are the additive (Sb of 1.0-3.0 weight part (preferred 1.5-2.5 weight part, more preferably 2.2 weight parts)
2O
3, ZnO and Pr
6O
11), account for SnO
2The SnO of the residue 65～35wt% of the total consumption of powder (preferred 60～40%, more preferably 50wt%)
2Powder, and then add 60～40 weight parts (for example 50 weight parts) (for example diameter is 8-12mm, preferred 10mm) water of zirconium oxide balls and 35～10 weight parts (for example 20 or 10 weight parts), sealing mixing and ball milling 2～30 hours (preferred 3～20 hours, more preferably 4～15 hours);
2) drying;
3) pulverize;
4) cold isostatic compaction;
5) optional base substrate is repaired: repair billet surface smooth;
6) sintering.
In the 3rd embodiment based on second embodiment of the present invention, the preparation method of stannic oxide electrode ceramic material is provided, it comprises the steps:
1) ball milling processing:
According to following material rate weighing: the SnO of 100 weight parts
2Powder (mean particle size 5～0.5 μ m), the Sb of 0.5～1.5 weight part (preferred 0.6～1.3, more preferably 0.7～1.1)
2O
3(mean particle size 5～0.5 μ m), the ZnO (mean particle size 5～0.5 μ m) of 0.1～1.5 weight part (preferred 0.6～1.3, more preferably 0.7～1.1), the Pr of 0.1～1.5 weight part (preferred 0.2～1.1, more preferably 0.3～0.8)
6O
11(mean particle size 5～0.5 μ m), wherein Sb
2O
3, ZnO and Pr
6O
11The weight summation be 1.0-3.0 weight part (preferred 1.5-2.5 weight part, more preferably 2.2 weight parts), the sodium silicate aqueous solution (preferably its degree Beaume is in 49～55% scopes) of 0.05～0.5 weight part (preferred 0.1～0.4, more preferably 0.15～0.3);
Mechanical milling process: above 0.1～1.0 weight part sodium silicate aqueous solution of having got ready is dissolved in or be blended in the water of 20-40 weight part (for example 25 or 35 weight parts) after join in the ball mill, then (for example diameter is 8-12mm, preferred 10mm) zirconium oxide balls of 40～60 weight parts (for example 50 weight parts) is added in the ball milling; Preferably, requiring various additives (is Sb
2O
3, ZnO and Pr
6O
11) and SnO
2The part by weight of powder and abrading-ball is 1: 0.9～2.0 (preferred 1: 1.2～1.6)), adding accounts for SnO respectively then
2The SnO of 35～65wt% of the total consumption of powder (i.e. 100 weight parts) (preferred 40～60%, more preferably 50wt%)
2Additive (the Sb of powder, whole consumption (1.0-3 weight part, preferred 1.5-2.5 weight part, more preferably 2.2 weight parts)
2O
3, ZnO and Pr
6O
11), account for SnO
2The SnO of the residue 65～35wt% of the total consumption of powder (preferred 60～40%, more preferably 50wt%)
2Powder, and then add 60～40 weight parts (for example 50 weight parts) (for example diameter is 8-12mm, preferred 10mm) water of zirconium oxide balls and 40～20 weight parts (for example 35 or 25 weight parts), sealing mixing and ball milling 2～30 hours (preferred 3～20 hours, more preferably 4～15 hours);
2) drying;
3) pulverizing: with step 2) the dried mixed powder that obtains grinds, and crosses the opening sieve of 25-35 order (preferred 30 orders (600 μ m)), obtains uniform mixed powder; Preferably, detect (pressing GB/T 3007-2006) powder moisture this moment less than 0.5wt%);
4) cold isostatic compaction: powder is incorporated with in the punching block of gum cover, the pressure pressurize of 200～250MPa 3～10 minutes, press base substrate;
5) optional base substrate is repaired: repair billet surface smooth;
6) do not have to press the neutral atmosphere sintering: base substrate is packed into calcined in 3～20 hours through 1450～1550 ℃ of insulations in the sintering oven, make high-purity stannic oxide electrode ceramic material of the present invention.
In step 1) in general, ball milling can be with inorganic corundum matter ball grinder.
Preferably, in first or second embodiment, wherein in step 2) in drying be following operation: with mixed slurry in Electric heat oven more than 120 ℃ temperature baking pulverize back sampling Detection (pressing GB/T 3007-2006) moisture preferably less than 0.5% more than 14 hours.
Preferably, in the present invention and special satisfy following technical indicator as the tindioxide powder of raw material in an embodiment:
SnO
2〉=99.5%; Cu≤3PPM; Fe≤150PPM; Pb≤140PPM; Burn and lose≤0.025%; Whiteness 〉=84.5; The SnO that ratio 98wt% is above
2The mean particle size of powder＜5 μ m).
As sodium silicate aqueous solution, use degree Beaume in 49～55% scopes, more preferably in 50～54% scopes, the more preferably sodium silicate aqueous solution in 51～53% scopes.
Advantage of the present invention: the advantage of this high-purity stannic oxide electrode ceramic material is to glass non-coloring, high temperature resistant.Using sintering aid is ZnO, Pr
6O
11Deng.
Resistance and resistivity that the temperature-raising method resistance furnace is measured the tin oxide electrode stupalith are all lower than the prior art, and iron level is less than or equal to 150ppm, and lead content is less than or equal to 140ppm, and copper content is less than 20ppm.
The use temperature of stannic oxide electrode ceramic material of the present invention can reach the temperature between 1500～1550 ℃.
Finally, the invention provides a kind of stannic oxide electrode ceramic material, its special type is that it comprises or is grouped into by following one-tenth: the SnO of 100 weight parts
2With Sb as 0.5～1.5 weight part of additive
2O
3, the ZnO of 0.1～1.5 weight part and the Pr of 0.1～1.5 weight part
6O
11, Sb wherein
2O
3, ZnO and Pr
6O
11The weight summation be 1.0-3.0 weight part and 0.05～0.5 weight part (preferred 0.1～0.4 weight part) water glass; Be that iron level is less than or equal to 150ppm, lead content is less than or equal to 140ppm, copper content is less than 20ppm.Detection method is an atomic absorption method.
Embodiment:
The present invention is further elaborated below in conjunction with specific embodiment, and these embodiment are just to illustrating the present invention, but do not limit protection scope of the present invention.Protection scope of the present invention is defined by the following claims.
Embodiment 1
According to following material rate weighing: the SnO of 10kg
2Powder (purity 99.6wt%, mean particle size 1 μ m), the Sb of 0.1kg
2O
3(purity 99.6wt%, mean particle size 1.5 μ m), the ZnO of 0.07kg (purity 99.6wt%, mean particle size 1.5 μ m), the Pr of 0.05kg
6O
11(purity 99.1wt%, mean particle size 1.2 μ m), the degree Beaume of 0.012kg is 52% sodium silicate aqueous solution; Wherein require the purity of raw material to be: SnO
2, purity 〉=99.5wt%; Sb
2O
3, purity 〉=99.5wt%; ZnO, purity 〉=99.5wt%; Pr
6O
11, purity 〉=99wt%;
The diameter of 5kg is added in the ball mill for the 10mm zirconium oxide balls, and then the degree Beaume that 0.012kg has been got ready is that 52% sodium silicate aqueous solution and 2kg water dissolve each other and joins in the ball mill, adds the SnO of 5kg afterwards respectively
2The additive of powder, the 0.22kg (Sb of 0.1kg
2O
3, the ZnO of 0.07kg and the Pr of 0.05kg
6O
11), add 5kgSnO again
2The diameter of powder and 5kg is 10mm zirconium oxide balls and 2kg water, seals mixing and ball milling then 6 hours;
Dry: with mixed slurry in Electric heat oven more than 120 ℃ the temperature baking detect moisture less than 0.3wt% by national standard (GB/T 3007-2006) more than 14 hours;
Pulverize: the opening that the blended powder was ground 30 orders (600 μ m) sieves, and obtains uniform mixed powder;
Cold isostatic compaction: the powder after the granulation is incorporated with in the punching block of gum cover, the pressure pressurize of 220MPa 7 minutes, press base substrate;
Base substrate finishing: repair billet surface smooth;
Do not have to press the neutral atmosphere sintering: base substrate is packed in the sintering oven through 1450 ℃ of insulations calcining in 5 hours, make high-purity stannic oxide electrode ceramic material of the present invention.
Embodiment 2:
Repeat the operation of embodiment 1, just, make high-purity stannic oxide electrode ceramic material of the present invention through 1500 ℃ of insulations calcining in 5 hours.
Embodiment 3:
Repeat the operation of embodiment 1, just, make high-purity stannic oxide electrode ceramic material of the present invention through 1550 ℃ of insulations calcining in 5 hours.
Embodiment 4:
Repeat the operation of embodiment 1, just make promoting agent with the sodium silicate aqueous solution of the degree Beaume 52% of 0.006kg, and SnO
2, Sb
2O
3, ZnO, Pr
6O
11Mass ratio be 1: 0.008: 0.005: 0.004, total consumption of these four kinds of raw materials is 1017g (additive is for adding), with 350ml water mixing and ball milling evenly, oven dry, grinding, moulding, make high-purity stannic oxide electrode ceramic material of the present invention through 1500 ℃ of insulations calcining in 5 hours.
Embodiment 5:
Repeat the operation of embodiment 1, just make promoting agent, press SnO with the sodium silicate aqueous solution of the degree Beaume 52% of 0.006kg
2, Sb
2O
3, ZnO, Pr
6O
11Mass ratio be 1: 0.008: 0.007: 0.003 weighing 1000g SnO
2And additive (Sb
2O
3, ZnO, Pr
6O
11) amount and 400ml water mixing and ball milling evenly, oven dry, grinding, moulding, make high-purity stannic oxide electrode ceramic material of the present invention through 1530 ℃ of insulations calcining in 5 hours.
The resistance of measuring the tin oxide electrode stupalith is the sample with 1*1*7cm, uses the conduction silver paste to connect sample and platinum wire lead-in wire.
The resistance of tin oxide electrode stupalith and resistivity
Physicals contrast: inspecting standard GB/T 2997-2000 (2004)
| Performance | The coventional type of prior art | Embodiment 1 | Embodiment 2 | Embodiment 5 |
| Apparent porosity (%) | ??≤1 | ??5 | ??4.9 | ??4.7 |
| Body close (volume density) (g/cm 3) | ??≥6.60 | ??6.30 | ??6.35 | ??6.20 |
| 1600 ℃ of cracking resistances | Difference | Excellent | Excellent | Excellent |
| Iron (Fe) content | ??＞200ppm | ??≤110ppm | ??≤105ppm | ??≤110ppm |
| Lead content | ??＞200ppm | ??≤100ppm | ??≤90ppm | ??≤105ppm |
| Copper content | ??＞50ppm | ??＜20ppm | ??＜20ppm | ??＜20ppm |
The stannic oxide electrode ceramic material that is obtained by method of the present invention has the following advantages:
1) improve the use temperature: former use temperature is 1350～1400 ℃; Present use temperature can be 1500～1550 ℃ of scopes;
2) reduce electrode normal temperature and high temperature resistance (temperature-raising method resistance furnace mensuration): referring to the subordinate list of front;
3) minimizing is painted to glassware: (contrast test heats up in the white glass material);
4) use that reaches simultaneously laser glass requires: laser glass requires iron content low, generally be lower than 500ppm, preferably be lower than 300ppm, more preferably less than 150ppm, again more preferably less than 50ppm, without copper and manganese, have copper then copper content be less than 20ppm. Detection method is that atom absorbs method.
Claims (9)
1. stannic oxide electrode ceramic material is characterized in that it comprises: the SnO of 100 weight parts
2With Sb as 0.5～1.5 weight part of additive
2O
3, the ZnO of 0.1～1.5 weight part and the Pr of 0.1～1.5 weight part
6O
11, Sb wherein
2O
3, ZnO and Pr
6O
11The weight summation be 1.0-3.0 weight part and 0.05～0.5 weight part water glass; Be that iron level is less than or equal to 150ppm, lead content is less than or equal to 140ppm, detection method is an atomic absorption method.
2. the preparation method of the stannic oxide electrode ceramic material of claim 1, it comprises the steps:
1) ball milling processing:
Mechanical milling process: 0.1～1.0 weight part sodium silicate aqueous solution is dissolved in or be blended in the water of 20-30 weight part after join in the ball mill, then add the SnO of 100 weight parts
2Powder and as the Sb of 0.5～1.5 weight part of additive
2O
3, the ZnO of 0.1～1.5 weight part and the Pr of 0.1～1.5 weight part
6O
11, Sb wherein
2O
3, ZnO and Pr
6O
11The weight summation be the 1.0-3.0 weight part, and then add the water of 30～20 weight parts, sealing mixing and ball milling 2～30 hours;
2) drying;
3) pulverize;
4) cold isostatic compaction;
5) optional base substrate is repaired: repair billet surface smooth;
6) sintering.
3. according to the method for claim 2, wherein mechanical milling process is following process:
Mechanical milling process: 0.1～1.0 weight part sodium silicate aqueous solution is dissolved in or be blended in the water of 20-30 weight part after join in the ball mill, then the zirconium oxide balls of 40～60 weight parts is added in the ball mill, add 35～65 weight parts then successively (based on the SnO of 100 weight parts
2The total consumption of powder) SnO
2Powder, the Sb of 0.5～1.5 weight part
2O
3, the ZnO of 0.1～1.5 weight part and the Pr of 0.1～1.5 weight part
6O
11, Sb wherein
2O
3, ZnO and Pr
6O
11The weight summation be the 1.0-3.0 weight part, add 65～35 weight parts again (based on the SnO of 100 weight parts
2The total consumption of powder) SnO
2Powder, and then add the zirconium oxide balls of 60～40 weight parts and the water of 30～20 weight parts, sealing mixing and ball milling 2～30 hours.
4. according to the method for claim 2 or 3, wherein the step 5) cold isostatic compaction is following carrying out:
Powder is incorporated with in the punching block of gum cover, pressurize is 3～10 minutes under the pressure of 200～250MPa, press base substrate.
5. according to the method for claim 2 or 3, wherein the step 6) sintering is following carrying out:
Base substrate is packed in the sintering oven through 1450～1550 ℃ of insulations calcining in 3～20 hours, make high-purity stannic oxide electrode ceramic material of the present invention.
6. according to any one method among the aforementioned claim 2-5, wherein the degree Beaume of sodium silicate aqueous solution is in 49～55% scopes.
7. the stannic oxide electrode ceramic material that obtains by the method for any one among the claim 2-6.
8. the stannic oxide electrode ceramic material of claim 7, its use temperature can reach the temperature between 1500～1550 ℃.
9. claim 7 or 8 stannic oxide electrode ceramic material, wherein iron level is less than or equal to 150ppm, and lead content is less than or equal to 140ppm, and copper content is less than 20ppm, and detection method is an atomic absorption method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101715450A CN101830694B (en) | 2010-05-06 | 2010-05-06 | High-purity stannic oxide electrode ceramic material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010101715450A CN101830694B (en) | 2010-05-06 | 2010-05-06 | High-purity stannic oxide electrode ceramic material and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101830694A true CN101830694A (en) | 2010-09-15 |
| CN101830694B CN101830694B (en) | 2013-12-11 |
Family
ID=42714938
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010101715450A Active CN101830694B (en) | 2010-05-06 | 2010-05-06 | High-purity stannic oxide electrode ceramic material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101830694B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104557017A (en) * | 2013-10-21 | 2015-04-29 | 湖北德睿四通科技有限公司 | Stannic oxide electrode ceramic material as well as preparation method thereof |
| CN114149258A (en) * | 2021-12-29 | 2022-03-08 | 全球能源互联网研究院有限公司 | Piezoelectric ceramic with laminated structure and preparation method and application thereof |
| CN114315341A (en) * | 2021-12-28 | 2022-04-12 | 广州市石基耐火材料厂 | Manganese-containing high-purity tin ceramic, preparation method thereof, manganese-containing high-purity tin brick and application |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060016223A1 (en) * | 2004-07-23 | 2006-01-26 | Saint-Gobain Ceramics & Plastics, Inc. | Tin oxide material with improved electrical properties for glass melting |
| CN1896320A (en) * | 2006-06-19 | 2007-01-17 | 哈尔滨工业大学 | Rare-earth doped titanium-base SnO2 electrolytic electrode and its preparation |
| CN101182096A (en) * | 2007-11-09 | 2008-05-21 | 东华大学 | Preparation method of tin oxide electrode for glass electric melting furnace |
| CN101439967A (en) * | 2008-12-26 | 2009-05-27 | 武汉理工大学 | Preparation of high compactness stannic oxide ceramic |
| CN101439966A (en) * | 2008-12-26 | 2009-05-27 | 武汉理工大学 | Preparation of stannic oxide electrode ceramic material |
-
2010
- 2010-05-06 CN CN2010101715450A patent/CN101830694B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060016223A1 (en) * | 2004-07-23 | 2006-01-26 | Saint-Gobain Ceramics & Plastics, Inc. | Tin oxide material with improved electrical properties for glass melting |
| CN1896320A (en) * | 2006-06-19 | 2007-01-17 | 哈尔滨工业大学 | Rare-earth doped titanium-base SnO2 electrolytic electrode and its preparation |
| CN101182096A (en) * | 2007-11-09 | 2008-05-21 | 东华大学 | Preparation method of tin oxide electrode for glass electric melting furnace |
| CN101439967A (en) * | 2008-12-26 | 2009-05-27 | 武汉理工大学 | Preparation of high compactness stannic oxide ceramic |
| CN101439966A (en) * | 2008-12-26 | 2009-05-27 | 武汉理工大学 | Preparation of stannic oxide electrode ceramic material |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104557017A (en) * | 2013-10-21 | 2015-04-29 | 湖北德睿四通科技有限公司 | Stannic oxide electrode ceramic material as well as preparation method thereof |
| CN104557017B (en) * | 2013-10-21 | 2019-01-04 | 湖北德睿四通科技有限公司 | A kind of stannic oxide electrode ceramic material and preparation method thereof |
| CN114315341A (en) * | 2021-12-28 | 2022-04-12 | 广州市石基耐火材料厂 | Manganese-containing high-purity tin ceramic, preparation method thereof, manganese-containing high-purity tin brick and application |
| CN114149258A (en) * | 2021-12-29 | 2022-03-08 | 全球能源互联网研究院有限公司 | Piezoelectric ceramic with laminated structure and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101830694B (en) | 2013-12-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104671771B (en) | A kind of high-voltage gradient zinc oxide base voltage sensitive resistor material and preparation method thereof | |
| CN101786873B (en) | Method for preparing electrolyte ceramic membrane of lithium ion battery | |
| CN103803968B (en) | Low-k low-temperature co-burning ceramic material and preparation method thereof in one | |
| CN101691297B (en) | Ferrite/ceramic composite material and preparation method and application thereof | |
| CN103693953B (en) | Middle and low voltage zinc oxide varistor and preparation method thereof | |
| CN101439966A (en) | Preparation of stannic oxide electrode ceramic material | |
| CN102354545A (en) | Sliver electrode slurry for back electric field of silicon solar cell and preparation method thereof | |
| CN104801709B (en) | Nickel-coated copper clad metal powder and preparation method and application thereof | |
| CN106676487B (en) | A kind of zinc oxide-based ceramic sputtering target material and its preparation method and application | |
| CN107473731A (en) | A kind of high-energy type piezo-resistance and its manufacture method | |
| CN105130193A (en) | Low-temperature matte reaction glaze and production method thereof | |
| CN104464882B (en) | A kind of photovoltaic cell silver slurry and sintering method thereof | |
| CN102234194B (en) | Ceramic material of stannic oxide electrode used for LCD (Liquid Crystal Display) glass and preparation method thereof | |
| CN103295659A (en) | Electrocondution slurry for solar cell and manufacturing method thereof | |
| CN101830694B (en) | High-purity stannic oxide electrode ceramic material and preparation method thereof | |
| CN109455940A (en) | A kind of soft lead-free low-temperature seal glass and preparation method thereof | |
| CN102875142A (en) | Preparation method of stannic oxide ceramic electrode | |
| CN108178615B (en) | Microwave ceramic dielectric sintered powder material, microwave dielectric ceramic and application thereof | |
| CN101948304B (en) | Preparation method of stannic oxide electrode | |
| KR102302205B1 (en) | Silver powder manufacturing method | |
| CN115667169A (en) | Preparation method of glass powder, silver paste and preparation method | |
| CN104404573A (en) | Preparation method of vanadium metal | |
| CN110467448B (en) | Preparation method of nano NTC ceramic powder suitable for tape casting and tape casting film | |
| CN105304242B (en) | A kind of preparation method of low B values high value thick film NTC slurries | |
| CN104465875B (en) | A kind of preparation method of photovoltaic cell silver grating line |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |