CN101003192B - Laminated composite diffusive intensified platinum and platinum alloy - Google Patents

Laminated composite diffusive intensified platinum and platinum alloy Download PDF

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Publication number
CN101003192B
CN101003192B CN200710065633A CN200710065633A CN101003192B CN 101003192 B CN101003192 B CN 101003192B CN 200710065633 A CN200710065633 A CN 200710065633A CN 200710065633 A CN200710065633 A CN 200710065633A CN 101003192 B CN101003192 B CN 101003192B
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platinum
lamination
strip
ingot blank
platinum alloy
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CN101003192A (en
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秦国义
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Abstract

A laminated and diffusion reinforced Pt, Pt-Au, or Pt-Rh material used to prepare crucible or leakage plate for preparing optical glass or glass fibers is made up of not less than 150 sheets through laminating and rolling. Said sheet is proportionally prepared from Pt or Pt-alloy and at least one of Zr, Y and Sc.

Description

Compound dispersion intensifying platinum of lamination and platinum alloy
Technical field:
The present invention relates to optical glass and glass fibre production with dispersion intensifying platinum and platinum alloy material.
Technical background:
In optical glass production, must use Pt or Pt-Au alloy to do the crucible material, in the production of glass fibre, must use the Pt-Rh alloy to make to leak fine drain board material.In order to improve the elevated temperature strength and the serviceability temperature of Pt, Pt-Au and Pt-Rh alloy, dispersion-strengtherning Pt, Pt-Au and Pt-Rh alloy crucible and drain board material have been invented.Dispersion-strengtherning Pt, the Pt-Au that is applied at present, Pt-Rh material mainly contain DPHPt, DPHPt-Au, DPHPt-Rh, ZGS Pt, ZGS Pt-Au, ZGS Pt-Rh, ODS Pt, ODS Pt-Au, ODS Pt-Rh.ZGS Pt, ZGS Pt-Au, ZGS Pt-Rh adopt ZrO to make disperse phase; ODS Pt, ODS Pt-Au, ODS Pt-Rh adopt Y 2O 3Make disperse phase; DPHPt, DPHPt-Au, DPHPt-Rh adopt ZrO and Y 2O 3, Sc 2O 3Make disperse phase Deng one or both combinations in the rare earth oxide.ZGS Pt, ZGS Pt-Au, ZGSPt-Rh, ODS Pt, ODS Pt-Au, ODS Pt-Rh material mainly adopt chemical codeposition legal system get everything ready Pt, Pt-Au, the Pt-Rh powder of disperse phase, then by powder compacting, sintering, forge and operation preparation such as rolling.Major defect is that the disperse phase particle can only reach micron order, tiny inadequately, distribute inadequately evenly, weldability is relatively poor, the weld high-temperature behavior is relatively poor, complex process, fabrication cycle are long, the manufacturing expense height; DPHPt, DPHPt-Au, DPHPt-Rh material preparation method are with a small amount of Zr, Y or other rare earth element and Pt, Pt-Au, Pt-Rh melting and casting, are rolled into 2~3 millimeters slabs, and then carry out in the high temperature pure oxygen atmosphere that oxidation obtains disperse phase in more than 100 hour, reroll at last and make finished product.Its major defect is internal oxidation furnaces requirement height, cost of equipment height; Interior oxidization time is long, and the sheet material core is difficult to realize interior oxidation, and the cycle is longer, and manufacturing expense is higher.
Summary of the invention:
Purpose of the present invention aims to provide that a kind of technology is simple, fabrication cycle is short, compound dispersion intensifying platinum of the lamination of low cost of manufacture and platinum alloy.
Another object of the present invention aims to provide the manufacture method of compound dispersion intensifying platinum of this lamination and platinum alloy.
Compound dispersion intensifying platinum of lamination of the present invention and platinum alloy, it is by being no less than rolling forming behind 150 the stack of sheets, thin slice is made of at least a and platinum and the platinum alloy among rare earth element Zr, Y and the Sc, wherein the percentage by weight of rare earth element Zr, Y and Sc is 0.02%~0.5%, and the thickness of thin slice is less than 0.5mm.Au content is 0.1~5% in the platinum alloy, Rh content is 1~20%.
Compound dispersion intensifying platinum of lamination of the present invention and platinum alloy, its preparation method may further comprise the steps:
A with 0.02%~0.5% Zr and rare earth elements such as Y, Sc one or more with Pt, Pt-Au, Pt-Rh in a vacuum frequently in the induction furnace founding become ingot blank;
B is rolled into strip below the 0.5mm to ingot blank;
C is oxidation in strip is in 900~1600 ℃ oxygen atmosphere stove more than 15 hours;
The strip of d after with interior oxidation is cut into and is wider than 30mm, grows up to be combined with each other in the 50mm small pieces and with 150 above small pieces laminations and form the thin layer composite ingot blank;
E is pressing the compound ingot blank of lamination knot, is forging the fine and close compound ingot blank of lamination more than 700 ℃;
F is at hot rolling deformation more than 700 ℃, and pass deformation is greater than 10%, and total heat distortion amount is greater than 40%;
The lamination composite plate of g after with hot rolling is cold rolled to makes crucible and glass bushing desired thickness gets final product.
The compound dispersion-strengtherning Pt of lamination, Pt-Au, Pt-Rb alloy that the present invention makes, the diffusing particle size is below 40 nanometers, than extremely when young more than 5 times of powder metallurgy process manufacturing, the spread, it is the granule number on the unit are, the raising of making than powder metallurgy process is more than 5 times, thereby its high-temperature behavior is significantly improved; Secondly, oxidation is compared with previous slab internal oxidation in the thin slice that the present invention adopts, do not exist in the weak oxide situation, oxidizing process of slab core diffusing particle can alligatoring, oxidation is complete, thereby its high-temperature behavior is apparently higher than the slab internal oxidation; In addition, the compound dispersion-strengtherning Pt of lamination, Pt-Au, Pt-Rh alloy have realized that the combination of dispersion-strengtherning and complex intensifying all further is significantly improved performances such as its processing characteristics, high-temperature behavior, punching press and welding, and this is that powder metallurgy process and slab internal oxidation can't be accomplished; At last, technology of the present invention is uncomplicated, the manufacturing cycle short, low cost of manufacture, has overcome the deficiency that powder metallurgy process and slab internal oxidation technology are complicated, the manufacturing cycle is long, manufacturing cost is high.
The present invention proposes a kind of new method and formation of making dispersion-strengtherning Pt, Pt-Au and Pt-Rh crucible, drain board material, effectively overcome the shortcoming that previous manufacturing dispersion-strengtherning Pt, Pt-Au, Pt-Rh method exist and dispersion-strengtherning Pt, Pt-Au, Pt-Rh combination property are significantly increased than previous method manufacturing.
The specific embodiment
The invention will be further described below by embodiment, but be not limited to embodiment.
Embodiment 1
With the Pt of 5000 gram purity 〉=99.95%, the Zr ZrO that packs into of 5 gram purity 〉=99.6% 2In the crucible, melting and water to cast from the flat mold and obtain ingot blank in the induction furnace frequently in a vacuum, with ingot blank rolling be the 0.2mm strip; Strip in atmospheric furnace in 1100 ℃ down in oxidation 70 hours, obtain dispersion-strengtherning Pt strip; Dispersion-strengtherning Pt strip is cut out the small pieces wide for 60mm, that 90mm is long and 200 are superimposed together, press knot, forge into fine and close billet in 900 ℃ then; At the fine and close billet of 900 ℃ of hot rollings, pass deformation is 20%, and total heat is deformed into 50%, is cold rolled to 0.8~1mm by 10% pass deformation then and promptly obtains the compound dispersion-strengtherning Pt of lamination crucible making sheet material.
Embodiment 2
With the Pt-5Au of 5000 gram purity 〉=99.95%, the Zr ZrO that packs into of 5 gram purity 〉=99.6% 2In the crucible, melting and water to cast from the flat mold and obtain ingot blank in the induction furnace frequently in a vacuum, with ingot blank rolling be the 0.2mm strip; Strip in atmospheric furnace in 1200 ℃ down in oxidation 70 hours, obtain dispersion-strengtherning Pt-5Au strip; Dispersion-strengtherning Pt-5Au strip cut out for 9cm is long, 6cm is wide small pieces and with 200 be superimposed together, press knot, forge into fine and close billet in 900 ℃ then; At the fine and close billet of 900 ℃ of hot rollings, pass deformation is 20%, and total heat is deformed into 50%, is cold rolled to 0.8~1mm by 10% pass deformation then and promptly obtains the compound dispersion-strengtherning Pt-5Au of lamination crucible making sheet material.
Embodiment 3
With the Pt-10Rh of 4990 gram purity 〉=99.95%, the Zr ZrO that packs into of 15 gram purity 〉=99.6% 2In the crucible, melting and water to cast from the flat mold and obtain ingot blank in the induction furnace frequently in a vacuum, with ingot blank rolling be the 0.2mm strip; Strip in atmospheric furnace in 1300 ℃ down in oxidation 70 hours, obtain dispersion-strengtherning Pt-10Rh strip; Dispersion-strengtherning Pt-10Rh strip cut out for 9cm is long, 6cm is wide small pieces and with 200 be superimposed together, press knot, forge into fine and close billet in 1000 ℃ then; At the fine and close billet of 1000 ℃ of hot rollings, pass deformation is 20%, and total heat is deformed into 50%, is cold rolled to 1.5~1.8mm by 10% pass deformation then and promptly obtains the compound dispersion-strengtherning Pt-10Rh of lamination drain board material.
Embodiment 4
With the Pt of 5003 gram purity 〉=99.95%, the Y ZrO that packs into of 10 gram purity 〉=99.6% 2In the crucible, melting and water to cast from the flat mold and obtain ingot blank in the induction furnace frequently in a vacuum, with ingot blank rolling be the 0.2mm strip; Strip in atmospheric furnace in 1100 ℃ down in oxidation 70 hours, obtain dispersion-strengtherning Pt strip; Dispersion-strengtherning Pt strip cut out for 90mm is long, 60mm is wide small pieces and with 180 be superimposed together, press knot, forge into fine and close billet in 1000 ℃ then; At the fine and close billet of 900 ℃ of hot rollings, pass deformation is 30%, and total heat is deformed into 70%, is cold rolled to 0.8~1mm by 10% pass deformation then and promptly obtains the compound dispersion-strengtherning Pt of lamination crucible making sheet material.
Embodiment 5
With Pt-5Au, the 5 gram Zr of purity 〉=99.6% of 5000 gram purity 〉=99.95% and the Y ZrO that packs into 2In the crucible, melting and water to cast from the flat mold and obtain ingot blank in the induction furnace frequently in a vacuum, with ingot blank rolling be the 0.3mm strip; Strip in atmospheric furnace in 1300 ℃ down in oxidation 80 hours, obtain dispersion-strengtherning Pt-5Au strip; Dispersion-strengtherning Pt-5Au strip is cut out the small pieces wide for 60mm, that 90mm is long and 200 are superimposed together, press knot, forge into fine and close billet in 1000 ℃ then; At the fine and close billet of 900 ℃ of hot rollings, pass deformation is 20%, and total heat is deformed into 50%, is cold rolled to 0.8~1mm by 10% pass deformation then and promptly obtains the compound dispersion-strengtherning Pt of lamination crucible making sheet material.
Embodiment 6
With Pt-3Au, the 10 gram Zr of purity 〉=99.6% of 4995 gram purity 〉=99.95% and the Sc ZrO that packs into 2In the crucible, melting and water to cast from the flat mold and obtain ingot blank in the induction furnace frequently in a vacuum, with ingot blank rolling be the 0.2mm strip; Strip in atmospheric furnace in 1200 ℃ down in oxidation 70 hours, obtain dispersion-strengtherning Pt-5Au strip; Dispersion-strengtherning Pt-5Au strip cut out for 9cm is long, 6cm is wide small pieces and with 200 be superimposed together, press knot, forge into fine and close billet in 1000 ℃ then; At the fine and close billets of 900 ℃ of hot rollings, pass deformation is 20%, and total heat is deformed into 50%, then by 10% pass deformation be cold rolled to~1mm promptly obtains the compound dispersion-strengtherning Pt-5Au of lamination crucible and makes and use sheet material.
Embodiment 7
With Pt-18Rh, 12 gram Zr, the Sc of purity 〉=99.6% of 4985 gram purity 〉=99.95% and the Y ZrO that packs into 2In the crucible, melting and water to cast from the flat mold and obtain ingot blank in the induction furnace frequently in a vacuum, with ingot blank rolling be the 0.2mm strip; Strip in atmospheric furnace in 1300 ℃ down in oxidation 70 hours, obtain dispersion-strengtherning Pt-10Rh strip; Dispersion-strengtherning Pt-10Rh strip cut out for 9cm is long, 6cm is wide small pieces and with 200 be superimposed together, press knot, forge into fine and close billet in 1000 ℃ then; At the fine and close billet of 1000 ℃ of hot rollings, pass deformation is 20%, and total heat is deformed into 50%, is cold rolled to 1.5~1.8mm by 10% pass deformation then and promptly obtains the compound dispersion-strengtherning Pt-10Rh of lamination drain board material.

Claims (4)

1. compound dispersion intensifying platinum of lamination and platinum alloy, it is characterized in that it is by being no less than rolling forming behind 150 the stack of sheets, thin slice is made of at least a and platinum and the platinum alloy among rare earth element Zr, Y and the Sc, wherein the percentage by weight of rare earth element Zr, Y and Sc is 0.02%~0.5%, and the thickness of thin slice is less than 0.5mm.
2. compound dispersion intensifying platinum of lamination according to claim 1 and platinum alloy is characterized in that in the described platinum alloy that the weight percent content of Au is 0.1~5%.
3. compound dispersion intensifying platinum of lamination according to claim 1 and platinum alloy is characterized in that in the described platinum alloy that the weight percent content of Rh is 1~20%.
4. the preparation method of compound dispersion intensifying platinum of lamination and platinum alloy is characterized in that its preparation method may further comprise the steps:
A becomes ingot blank with a kind of among at least a and Pt, the Pt-Au of 0.02%~0.5% Zr and Y, Sc rare earth element, Pt-Rh founding in vaccum sensitive stove;
B is rolled into strip below the 0.5mm to ingot blank;
C is oxidation in strip is in 900~1600 ℃ oxygen atmosphere stove more than 15 hours;
The strip of d after with interior oxidation is cut into and is wider than 30mm, grows up to be combined with each other in the 50mm small pieces and with 150 above small pieces laminations and form the thin layer composite ingot blank;
E is pressing the compound ingot blank of lamination knot, is forging the fine and close compound ingot blank of lamination more than 700 ℃;
F is at hot rolling deformation more than 700 ℃, and pass deformation is greater than 10%, and total heat distortion amount is greater than 40%;
The lamination composite plate of g after with hot rolling is cold rolled to makes crucible and glass bushing desired thickness gets final product.
CN200710065633A 2007-01-24 2007-01-24 Laminated composite diffusive intensified platinum and platinum alloy Expired - Fee Related CN101003192B (en)

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CN101984105A (en) * 2010-10-27 2011-03-09 贵研铂业股份有限公司 Method of preparing lamination dispersion strengthening platinum-base composite material
CN102952959B (en) * 2012-11-16 2014-07-02 无锡英特派金属制品有限公司 Composite dispersion strengthened platinum material production method
CN102936667B (en) * 2012-11-16 2014-05-07 无锡英特派金属制品有限公司 Preparation method of dispersed strengthened platinum rhodium and platinum composite material
KR102205156B1 (en) * 2013-10-23 2021-01-20 에이지씨 가부시키가이샤 Conduit for glass melt, container for glass melt, method for producing same, glass article production device, and glass article production method
CN105256167B (en) * 2015-10-09 2017-05-17 内江至诚铂业科技有限公司 Preparation method for platinum-rhodium alloy bushing plate base plate material
CN108251682A (en) * 2017-12-27 2018-07-06 南京悠谷新材料科技有限公司 A kind of preparation method of platinum magnesium metallic composite
CN110421004B (en) * 2019-07-30 2020-08-04 江西理工大学 Preparation method of aluminum oxide dispersion strengthened copper large plate belt material
EP3971311B1 (en) * 2020-09-17 2022-07-06 Heraeus Deutschland GmbH & Co. KG Improved dispersion-hardened precious metal alloy

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US4348216A (en) * 1980-10-27 1982-09-07 Owens-Corning Fiberglas Corporation Method and apparatus for forming glass fibers
CN1526546A (en) * 2003-09-23 2004-09-08 贵研铂业股份有限公司 Composit Pd-containing material wire and its prepn and use

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