JP2743982B2 - Black quartz glass foam and method for producing the same - Google Patents
Black quartz glass foam and method for producing the sameInfo
- Publication number
- JP2743982B2 JP2743982B2 JP4137703A JP13770392A JP2743982B2 JP 2743982 B2 JP2743982 B2 JP 2743982B2 JP 4137703 A JP4137703 A JP 4137703A JP 13770392 A JP13770392 A JP 13770392A JP 2743982 B2 JP2743982 B2 JP 2743982B2
- Authority
- JP
- Japan
- Prior art keywords
- quartz glass
- black
- foam
- powder
- temperature
- 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.)
- Expired - Fee Related
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C11/00—Multi-cellular glass ; Porous or hollow glass or glass particles
- C03C11/007—Foam glass, e.g. obtained by incorporating a blowing agent and heating
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Glass Compositions (AREA)
Description
【０００１】[0001]
【産業上の利用分野】本発明は、黒色石英ガラス発泡体
に関し、更に詳しくは、遠赤外線の放射体として有用な
高純度黒色石英ガラス発泡体及びその効果的製造方法に
関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a black quartz glass foam, and more particularly to a high-purity black quartz glass foam useful as a far-infrared radiator and a method for effectively producing the same.
【０００２】[0002]
【従来の技術】従来、石英ガラスの黒色化は、石英ガラ
ス中に五酸化バナジウム（Ｖ2Ｏ5）や三二酸化鉄（Ｆe2
Ｏ3）のような金属酸化物を呈色材として加えることに
よって行われている。しかし、これらの金属酸化物類に
よる黒色石英ガラスの発泡は、ガラスのアンモニア化反
応とそのガス離脱を利用する方法では、それぞれの高温
熱処理において、その発泡化の程度をコントロ−ルする
ことが容易でなく、更に黒色が茶褐色に変色したり発泡
体強度が低下するなどの不都合が避けられなかった。ま
た、それらの着色用金属類は比較的多量に含まれるの
で、半導体工業分野での熱処理用石英ガラス部材として
は好ましい素材ではなかった。2. Description of the Related Art Conventionally, blackening of quartz glass has been carried out by means of vanadium pentoxide (V 2 O 5 ) or iron sesquioxide (Fe 2
It is performed by adding a metal oxide such as O 3 ) as a coloring material. However, the foaming of black quartz glass by these metal oxides can be easily controlled by the high temperature heat treatment by a method utilizing the ammoniating reaction of the glass and the desorption of the gas. In addition, inconveniences such as discoloration of black to brown and reduced strength of the foam were unavoidable. Further, since these coloring metals are contained in a relatively large amount, they are not preferable materials for a quartz glass member for heat treatment in the semiconductor industry.
【０００３】また、近年、熱の利用において、遠赤外線
領域の熱放射が各種の分野において利用されるようにな
った。一方、これに関連して、石英ガラスは、その光学
的特性上、赤外部はよく通すが遠赤外領域への波長の変
換は少ないものであった。更に、これまでの黒色ガラス
は、金属酸化物粉体を石英もしくは石英ガラス粉体と混
合してガラス化して製造されているが、その混合物が不
均一になり易いため均質な黒色石英ガラスが得難く、特
に、高温熱処理による均質な発泡多孔質体の製造は困難
であった。In recent years, in the use of heat, heat radiation in the far infrared region has been used in various fields. On the other hand, in relation to this, quartz glass has a good ability to pass through the infrared region due to its optical characteristics, but has little conversion of the wavelength to the far infrared region. Furthermore, black glass so far has been manufactured by mixing a metal oxide powder with quartz or quartz glass powder and vitrifying it. However, the mixture tends to be non-uniform, so that a homogeneous black quartz glass is obtained. It is difficult, especially, to produce a homogeneous foamed porous body by high-temperature heat treatment.
【０００４】本発明者は、上記のような金属酸化物類に
よる石英ガラスの黒色発泡化の実状に鑑み、そのような
不都合を伴わない均質な黒色石英ガラス発泡体の製造法
を見出すべく、特に黒色化剤に着目して、多くの無機物
質について黒色化実験を行った結果、極めて実用的に望
ましい方法を開発した。[0004] In view of the fact that quartz glass is black foamed by metal oxides as described above, the present inventor has specifically sought to find a method for producing a homogeneous black quartz glass foam without such inconveniences. As a result of conducting blackening experiments on many inorganic substances, focusing on the blackening agent, an extremely practically desirable method was developed.
【０００５】[0005]
【発明が解決しようとする課題】従って、本発明の課題
は、Ｖ2Ｏ5やＦe2Ｏ3等の金属酸化物黒色化剤のような
高温熱履歴によって変色することがなく、強度の低下も
ない黒色石英ガラス発泡体を提供することにある。ま
た、他の課題は、遠赤外線放射率の優れた均質な黒色石
英ガラス発泡体を提供することにある。その他の課題な
いし目的は、以下の記載から一層明らかになるであろ
う。SUMMARY OF THE INVENTION Accordingly, an object of the present invention is to prevent discoloration due to a high-temperature heat history such as a metal oxide blackening agent such as V 2 O 5 and Fe 2 O 3 , and to reduce strength. The object of the present invention is to provide a black quartz glass foam which does not have any. Another object is to provide a homogeneous black quartz glass foam having excellent far-infrared emissivity. Other problems or objects will become more apparent from the following description.
【０００６】[0006]
【課題を解決するための手段】すなわち、本発明は、炭
素を１〜５重量％含有し、0.1〜1.5ｇ／ｃｍ3の見掛け
密度及び0.9以上の平均放射率を有する黒色石英ガラス
発泡体及びその効果的製造方法、すなわち、粒子径が0.
1〜1000μｍφの石英ガラス粉体に炭素形成先駆物質液
を加えて混合し、乾燥，粉砕した後、これを不活性ガス
雰囲気中で加熱して該炭素形成先駆物質を炭化させ、次
いで、得られた黒色組成物を所定形状の容器に入れて、
750〜1200℃の温度で石英ガラスをアンモニアと反応さ
せた後、更に、これを1400〜1700℃の温度に加熱して発
泡させることを特徴とする黒色石英発泡体の製造方法を
提案するものである。That is, the present invention provides a black quartz glass foam containing 1 to 5% by weight of carbon, having an apparent density of 0.1 to 1.5 g / cm 3 and an average emissivity of 0.9 or more; Its effective production method, i.e., the particle size is 0.
A carbon-forming precursor liquid is added to quartz glass powder having a diameter of 1 to 1000 μm, mixed, dried and pulverized, and then heated in an inert gas atmosphere to carbonize the carbon-forming precursor. Put the black composition in a container of a predetermined shape,
After reacting the quartz glass with ammonia at a temperature of 750 to 1200 ° C., it further proposes a method for producing a black quartz foam, characterized by heating it to a temperature of 1400 to 1700 ° C. to foam it. is there.
【０００７】本発明の方法においては、用いられる石英
ガラス粉体は、高純度のものであればよく、特に、四塩
化けい素を酸水素火炎中で加水分解して得られる石英ガ
ラス粉及びシリコンアルコキシドを加水分解して得られ
る石英ガラス粉等の合成石英ガラス粉体が好都合に用い
られる。これらは、要すれば、粉砕して粒子径が0.1〜1
000μｍに調整されるが、500μｍ以下にすることが望ま
しい。[0007] In the method of the present invention, the quartz glass powder used may be of high purity, particularly quartz glass powder and silicon powder obtained by hydrolyzing silicon tetrachloride in an oxyhydrogen flame. Synthetic quartz glass powder such as quartz glass powder obtained by hydrolyzing alkoxide is conveniently used. If necessary, these may be ground to a particle size of 0.1 to 1
It is adjusted to 000 μm, but is desirably 500 μm or less.
【０００８】次に、この石英ガラス粉体は炭素粉末と混
合されるが、単に両粉末を混合するのではなく、まず石
英ガラス粉体に強固に結合し得る炭素形成先駆物質の水
溶液を加え混和し乾燥させて、該物質を粉体表面に均一
に附着させた後、これを加熱して炭素化させ、粉砕して
石英ガラスと炭素の分離する恐れのない均一な微粉状組
成物に調製される。Next, the quartz glass powder is mixed with the carbon powder. Instead of simply mixing the two powders, first, an aqueous solution of a carbon-forming precursor capable of being strongly bonded to the quartz glass powder is added and mixed. After drying, the substance is uniformly adhered to the powder surface, and then heated to carbonize and pulverized to prepare a uniform fine powder composition without fear of separation of quartz glass and carbon. You.
【０００９】そのような微粉状組成物の製造に用いられ
る炭素形成先駆物質は、その溶液が石英ガラスに対して
親和性を有し、脱溶剤後及び炭化後にも強固に附着する
有機物であれば制限はいが、水溶液として提供される結
合材が好ましく、例えば、ポリビニルアルコ−ルのよう
な糊剤が実用的に有利に使用される。その結合剤は、例
えば、１〜５％程度の水溶液に調整して石英ガラス粉体
に加えられる。その添加量は、遠赤外線放射率と関連
し、炭素化によって１〜５重量％の範囲の所望炭素含有
量に応じて選択される。炭素含有量が１重量％未満では
石英ガラス発泡体が黒色ではなく灰色を呈し、放射率も
無色の石英ガラス発泡体並に低くなり、また、５重量％
を超えると３〜30μｍの波長の光の放射率が、0.9より
小さくなるので好ましくない。好ましい炭素含有量は、
1.5〜３重量％である。[0009] The carbon-forming precursor used in the production of such a finely powdered composition is an organic substance whose solution has an affinity for quartz glass and which adheres firmly even after solvent removal and carbonization. Although not restricted, a binder provided as an aqueous solution is preferable, and a sizing agent such as polyvinyl alcohol is practically and advantageously used. The binder is adjusted to, for example, an aqueous solution of about 1 to 5% and added to the quartz glass powder. The amount added is related to the far-infrared emissivity and is selected depending on the desired carbon content in the range of 1 to 5% by weight by carbonization. When the carbon content is less than 1% by weight, the quartz glass foam has a gray color instead of black, and the emissivity is as low as the colorless quartz glass foam, and 5% by weight.
Exceeding this is not preferable because the emissivity of light having a wavelength of 3 to 30 μm becomes smaller than 0.9. The preferred carbon content is
1.5 to 3% by weight.
【００１０】結合剤先駆物質の水溶液を石英ガラス粉に
均一に混合した組成物は、例えば、薄く広いバットに10
mmぐらいの厚さに広げて、50〜80℃程度の比較的低い温
度でまず乾燥処理される。その際、バットに広げないで
造粒機を用いて、100〜1000μm程度の粒径に造粒し乾燥
してもよい。次いで、乾燥された結合剤附着石英ガラス
粉体は、ボ−ルミル等で微粉末に粉砕され、非酸化性雰
囲気、例えば、窒素ガス雰囲気中で600〜1000℃の温度
に３〜８時間加熱処理して、有機結合剤を分解炭化させ
る。この炭化処理において炭素形成先駆物質中の炭素成
分は、温度その他の条件によって異なるが、通常、過半
量以上が炭素として残留し、得られた炭素含有ガラス粉
末は、純黒色ではなく濃い灰色である。A composition in which an aqueous solution of a binder precursor is uniformly mixed with quartz glass powder is applied, for example, to a thin and wide vat.
It is spread to a thickness of about mm and first dried at a relatively low temperature of about 50 to 80 ° C. At this time, the particles may be granulated to a particle size of about 100 to 1000 μm using a granulator without being spread over the vat, and dried. Next, the dried silica glass powder with a binder is pulverized into a fine powder by a ball mill or the like, and heat-treated at a temperature of 600 to 1000 ° C. for 3 to 8 hours in a non-oxidizing atmosphere, for example, a nitrogen gas atmosphere. Then, the organic binder is decomposed and carbonized. In this carbonization treatment, the carbon component in the carbon-forming precursor varies depending on the temperature and other conditions, but usually, a majority or more remains as carbon, and the resulting carbon-containing glass powder is not pure black but dark gray .
【００１１】得られた炭素含有石英ガラス粉体は、次い
でアンモニア化及び発泡体化処理される。両処理はいず
れも加熱反応であって、連続操作することができるの
で、例えば、該粉体の所定量を所望の発泡成形体に対応
する形状の容器に充填し、アンモニアガス雰囲気中で80
0〜1000℃の温度に３〜８時間保って反応させ、ガラス
中のＯＨ基をアンモニア化させる。このアンモニア化反
応温度が、800℃より低いと反応速度が遅く、また1300
℃を超えると形成された気泡が破壊されるので不都合で
ある。このアンモニア化におけるアンモニアガスの反応
区域への導入は、通常、窒素ガスをキャリアガスとして
適当な濃度に希釈して行われる。[0011] The obtained carbon-containing quartz glass powder is then subjected to ammoniating and foaming. Since both treatments are heating reactions and can be operated continuously, for example, a predetermined amount of the powder is filled in a container having a shape corresponding to a desired foamed molded product, and the powder is charged in an ammonia gas atmosphere.
The reaction is carried out at a temperature of 0 to 1000 ° C. for 3 to 8 hours, and the OH groups in the glass are ammoniated. If the ammoniating reaction temperature is lower than 800 ° C., the reaction rate is slow, and 1300
If the temperature exceeds ℃, the formed bubbles are destroyed, which is inconvenient. The introduction of ammonia gas into the reaction zone in this ammoniation is usually carried out by diluting nitrogen gas to a suitable concentration as a carrier gas.
【００１２】アンモニア化処理された炭素含有石英ガラ
ス粉体は、その雰囲気からアンモニアを除いて非酸化性
雰囲気下又は減圧下に、更に1500〜1700℃の温度に昇温
して通常、１〜５時間加熱して発泡化され、所望形状の
黒色石英ガラス発泡体に成形される。この発泡化温度が
1500℃未満では発泡速度が遅いので実用的でなく、ま
た、1700℃を超えると生じた気泡が破裂して独立気泡が
急激に少なくなり、強度の低下を招くので好ましくな
い。その好適温度範囲は、雰囲気の圧力条件によって多
少異なるが、1600〜1650℃である。The ammonia-treated carbon-containing quartz glass powder is heated to a temperature of 1500 to 1700 ° C. in a non-oxidizing atmosphere or under reduced pressure, except for removing ammonia from the atmosphere, usually to a temperature of 1 to 5 ° C. It is foamed by heating for a time and molded into a black quartz glass foam having a desired shape. This foaming temperature
If the temperature is lower than 1500 ° C., the foaming rate is low, so that it is not practical. On the other hand, if the temperature exceeds 1700 ° C., the generated bubbles burst, and the number of closed cells rapidly decreases, which is not preferable because the strength decreases. The preferred temperature range is 1600 to 1650 ° C., although it varies somewhat depending on the atmospheric pressure conditions.
【００１３】[0013]
【作用】このようにして合成石英ガラス及び炭素形成先
駆物質から誘導され形成された黒色石英ガラス発泡体
は、金属不純物類、例えば、Ｎa，Ｋ，Ｌi，Ａl，Ｆeや
Ｖなどを実質的に含まない高純度の石英ガラス黒色発泡
体であって、しかも酸化雰囲気下で加熱してもその黒色
が褪色あるいは変色することがなく、得られた黒色発泡
体は、軽量且つ優れた耐熱強度を有し、半導体工業にお
ける遠赤外線放射用部材として特に高い実用性を有す
る。The black quartz glass foam formed and derived from the synthetic quartz glass and the carbon-forming precursor in this manner substantially eliminates metal impurities such as Na, K, Li, Al, Fe, V, and the like. It is a high-purity quartz glass black foam that does not contain, and its black color does not fade or discolor even when heated in an oxidizing atmosphere, and the obtained black foam has light weight and excellent heat resistance. In addition, it has particularly high practicality as a member for far-infrared radiation in the semiconductor industry.
【００１４】[0014]
【実施例】次に、本発明を具体例により、更に詳細に説
明する。 実施例 １ 四塩化けい素（ＳiＣl4）を酸水素バ−ナ−に供給し
て、その火炎中で加水分解させて平均粒径約0.5μｍの
高純度石英ガラス粉体を作成した。この粉体500ｇにポ
リビニルアルコ−ルの３％水溶液1.3ｋｇを加えて撹拌
混合し、均一なスラリ−を調製した。このスラリ−をプ
ラスチック製平バットに約１ｃｍの厚さに広げて、70℃
に設定した恒温乾燥機中で24時間乾燥した。Now, the present invention will be described in further detail with reference to specific examples. Example 1 Silicon tetrachloride (SiCl 4 ) was supplied to an oxyhydrogen burner and hydrolyzed in the flame to produce a high-purity quartz glass powder having an average particle size of about 0.5 μm. To 500 g of this powder, 1.3 kg of a 3% aqueous solution of polyvinyl alcohol was added and mixed with stirring to prepare a uniform slurry. Spread this slurry on a plastic flat bat to a thickness of about 1 cm,
Was dried for 24 hours in a constant-temperature dryer set to.
【００１５】次いで、その乾燥粉体を合成石英ガラス内
張りのボ−ルミルで粉砕した。目開き1000μmのナイロ
ン篩をパスし、且つ目開き106μmのナイロン篩に残る粒
度範囲の粉体350ｇを石英ボ−トに移し、石英管状の炉
に入れ、窒素ガスを５リットル／分の割合で連続的に送
り込みながら、800℃の温度に５時間加熱処理して灰色
の粉体を得た。Next, the dried powder was pulverized with a ball mill lined with synthetic quartz glass. 350 g of powder having a particle size range passing through a nylon sieve having an opening of 1000 μm and passing through a nylon sieve having an opening of 106 μm is transferred to a quartz boat, placed in a quartz tubular furnace, and supplied with nitrogen gas at a rate of 5 l / min. While continuously feeding, a heat treatment was performed at a temperature of 800 ° C. for 5 hours to obtain a gray powder.
【００１６】次に、この粉体を再び石英管状炉内に入
れ、窒素ガスをキャリアガスとして10リットル／分の割
合で導入し、炉内の温度が850℃になったところでアン
モニアガスを２ルットル／分の割合でキャリアガスに混
合して送り込んだ。この状態を５時間保持してアンモニ
ア化反応を行わせた。続いて、両ガスの供給を止め、炉
内をの温度を1650℃に上げて減圧下に３時間保持し、反
応ガスを離脱させて黒色の石英ガラス発泡体を得た。そ
の発泡体の密度は、1.1ｇ／cm3であった。Next, the powder is put again into a quartz tube furnace, and nitrogen gas is introduced as a carrier gas at a rate of 10 liter / min. When the temperature in the furnace reaches 850 ° C., ammonia gas is added at 2 liters. / Minute and mixed with the carrier gas and sent. This state was maintained for 5 hours to carry out the ammoniaation reaction. Subsequently, the supply of both gases was stopped, the temperature inside the furnace was raised to 1650 ° C., and the pressure was maintained under reduced pressure for 3 hours, and the reaction gas was released to obtain a black quartz glass foam. The density of the foam was 1.1 g / cm 3 .
【００１７】得られた黒色石英ガラス発泡体は、炭素含
有量が約2.5重量％で、不純物として含まれるＮa，Ｋ，
Ｌi，Ａl，Ｆe及びＶは、いずれも金属として0.1ppm以
下であった。また、その黒色発泡体の遠赤外線（３〜30
μｍ）放射率を測定したところ0.91であった。これに対
し、着色剤を加えない無色透明の合成石英ガラス、及び
その発泡体の放射率は、それぞれ0.82及び0.83であっ
た。また、五酸化バナジウム1000ppmにより着色された
黒色石英ガラスの放射率は0.91であったが、そのガラス
中には、Ｎa：2.3ppm，Ｋ：1.6ppm，Ｌi：2.4ppm，Ａ
l：18ppmが含まれ、大気中での1000℃，10時間の加熱耐
酸化性試験において、やや脆くなることが認められた。The black quartz glass foam thus obtained has a carbon content of about 2.5% by weight and contains Na, K,
Li, Al, Fe and V were all less than 0.1 ppm as metal. In addition, far infrared rays (3 to 30) of the black foam
μm) The emissivity was measured to be 0.91. On the other hand, the emissivities of the colorless and transparent synthetic quartz glass to which no coloring agent was added and the foam thereof were 0.82 and 0.83, respectively. The emissivity of black quartz glass colored with 1000 ppm of vanadium pentoxide was 0.91, but the glass contained Na: 2.3 ppm, K: 1.6 ppm, Li: 2.4 ppm, A
l: Contains 18 ppm, and was found to be slightly brittle in a heat oxidation resistance test at 1000 ° C. for 10 hours in the atmosphere.
【００１８】実施例 ２ けい酸エチル2000ｇに蒸留水600ｇ，エチルアルコ−ル1
900ｇ及び１Ｎ規定塩酸270ccを加え、これをラウリン酸
150ｇを溶解したシクロヘキサン15ｋｇ中に注加して激
しく撹拌し、平均粒径30μmの石英粉600ｇの未乾燥粉末
を得た。この粉末500ｇを管状炉に入れ、炉内に窒素ガ
スを３リットル／分の速度で流しながら、炉内を10℃／
分の昇温速度で加熱し、800℃になってからその温度に
４時間保持して熱処理し、黒色の球状粉末420ｇを得
た。この黒色球状粉末20ｇを大気雰囲気下で600℃の温
度に５時間酸化処理したところ、19.4ｇに減少した。こ
の粉末には、炭素が約３重量％含まれることが確かめら
れた。EXAMPLE 2 600 g of distilled water and 2000 g of ethyl alcohol were added to 2000 g of ethyl silicate.
Add 900 g and 270 cc of 1N hydrochloric acid, and add
The solution was poured into 15 kg of cyclohexane in which 150 g was dissolved, and vigorously stirred to obtain 600 g of undried powder of quartz powder having an average particle size of 30 μm. 500 g of this powder was placed in a tube furnace, and nitrogen gas was flowed into the furnace at a rate of 3 liter / min.
And heated at 800 ° C. for 4 hours, followed by heat treatment to obtain 420 g of black spherical powder. When 20 g of this black spherical powder was oxidized at a temperature of 600 ° C. for 5 hours in an air atmosphere, it was reduced to 19.4 g. It was confirmed that this powder contained about 3% by weight of carbon.
【００１９】次いで、この黒色粉末を再び管状炉に入
れ、その炉内に窒素ガスをキャリアガスとして10リット
ル／分の割合で導入し、炉内の温度を850℃まで昇温さ
せた。この温度に達してから、更にアンモニアガスを３
リットル／分の割合で導入し、この状態に５時間保持し
て石英粉末のＯＨ基をアンモニアと反応させた。両ガス
の供給を止め、炉内を減圧下にして温度を1650℃に上
げ、その温度に３時間保って、密度が0.68ｇ／cm3黒色
石英ガラス発泡体を得た。この黒色石英発泡体の３〜30
μｍのいわゆる遠赤外線の放射率を測定したところ、0.
91であった。参考のために、この黒色発泡体15ｇを20％
ふっ化水素酸に溶解し、不溶の炭素をろ別乾燥してその
重量を測定したところ、0.435ｇであった。従って、黒
色石英発泡体中の炭素濃度は、約2.9％である。Next, the black powder was placed again in a tubular furnace, and nitrogen gas was introduced into the furnace at a rate of 10 liter / min as a carrier gas, and the temperature in the furnace was raised to 850 ° C. After reaching this temperature, add 3 more ammonia gases.
It was introduced at a rate of 1 liter / minute, and was kept in this state for 5 hours to react the OH groups of the quartz powder with ammonia. The supply of both gases was stopped, the temperature was raised to 1650 ° C. while the pressure in the furnace was reduced, and the temperature was maintained for 3 hours to obtain a black quartz glass foam having a density of 0.68 g / cm 3 . 3 ~ 30 of this black quartz foam
When the emissivity of so-called far-infrared light of μm was measured, it was found to be 0.
It was 91. For reference, 15g of this black foam is 20%
The powder was dissolved in hydrofluoric acid, and the insoluble carbon was separated by filtration and dried, and the weight was measured to be 0.435 g. Thus, the carbon concentration in the black quartz foam is about 2.9%.
【００２０】この発泡体を酸化雰囲気（大気）中に、10
00℃の温度に10時間保持したが、黒色に全く変化はなか
った。更に、より高い1350℃で２時間加熱したが、この
場合も変色，変形及び収縮は見られず、全く安定であっ
た。This foam is placed in an oxidizing atmosphere (air),
After being kept at a temperature of 00 ° C. for 10 hours, there was no change in black color. Further heating at a higher temperature of 1350 ° C. for 2 hours also showed no discoloration, deformation or shrinkage, and was completely stable.
【００２１】[0021]
【発明の効果】本発明の方法により得られる黒色石英ガ
ラス発泡体は、極めて均質で安定な色調を有し、高温酸
化条件下にも強度が低下しないばかりでなく、高い遠赤
外線放射率を有するので、半導体工業に極めて有用であ
る。The black quartz glass foam obtained by the method of the present invention has a very homogeneous and stable color tone, not only does not lose strength under high-temperature oxidation conditions, but also has a high far-infrared emissivity. Therefore, it is extremely useful in the semiconductor industry.
Claims (2)
／ｃｍ3の見掛け密度及び0.9以上の平均放射率を有する
黒色石英ガラス発泡体。1. A composition containing 1 to 5% by weight of carbon and 0.1 to 1.5 g
A black quartz glass foam having an apparent density of / cm 3 and an average emissivity of 0.9 or more.
粉体に炭素形成先駆物質液を加えて混合し、乾燥，粉砕
した後、これを不活性ガス雰囲気中で加熱して該炭素形
成先駆物質を炭化させ、次いで、得られた黒色組成物を
所定形状の容器に入れて、750〜1200℃の温度で石英ガ
ラスをアンモニアと反応させた後、更に、これを1400〜
1700℃の温度に加熱して発泡させることを特徴とする黒
色石英発泡体の製造方法。2. A carbon-forming precursor liquid is added to quartz glass powder having a particle diameter of 0.1 to 1000 μmφ, mixed, dried and pulverized, and then heated in an inert gas atmosphere to form the carbon-forming precursor. Then, the obtained black composition is placed in a container having a predetermined shape, and the quartz glass is reacted with ammonia at a temperature of 750 to 1200 ° C.
A method for producing a black quartz foam, characterized in that the foam is heated to a temperature of 1700 ° C. and foamed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4137703A JP2743982B2 (en) | 1992-04-30 | 1992-04-30 | Black quartz glass foam and method for producing the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4137703A JP2743982B2 (en) | 1992-04-30 | 1992-04-30 | Black quartz glass foam and method for producing the same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH05306142A JPH05306142A (en) | 1993-11-19 |
| JP2743982B2 true JP2743982B2 (en) | 1998-04-28 |
Family
ID=15204849
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4137703A Expired - Fee Related JP2743982B2 (en) | 1992-04-30 | 1992-04-30 | Black quartz glass foam and method for producing the same |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2743982B2 (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3793553B2 (en) * | 1999-03-31 | 2006-07-05 | 京セラ株式会社 | Black SiO2 corrosion-resistant member and method for producing the same |
| JP4540160B2 (en) * | 1999-12-27 | 2010-09-08 | 京セラ株式会社 | Black sintered quartz |
| JP2002075901A (en) * | 2000-08-31 | 2002-03-15 | Tokyo Electron Ltd | Annealer, plating system, and method of manufacturing semiconductor device |
| DE60324625D1 (en) | 2002-04-04 | 2008-12-24 | Tosoh Corp | Thermally sprayed quartz glass parts and manufacturing processes |
-
1992
- 1992-04-30 JP JP4137703A patent/JP2743982B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH05306142A (en) | 1993-11-19 |
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