JP2003192472A - Heat-resistant structure - Google Patents
Heat-resistant structureInfo
- Publication number
- JP2003192472A JP2003192472A JP2001393852A JP2001393852A JP2003192472A JP 2003192472 A JP2003192472 A JP 2003192472A JP 2001393852 A JP2001393852 A JP 2001393852A JP 2001393852 A JP2001393852 A JP 2001393852A JP 2003192472 A JP2003192472 A JP 2003192472A
- Authority
- JP
- Japan
- Prior art keywords
- heat
- resistant
- weight
- heat resistant
- coating layer
- 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
Landscapes
- Aftertreatments Of Artificial And Natural Stones (AREA)
- Furnace Housings, Linings, Walls, And Ceilings (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、例えば、焼成炉等
の炉壁に用いて好適な耐熱性構造体の改良に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to improvement of a heat resistant structure suitable for use in a furnace wall such as a baking furnace.
【０００２】[0002]
【従来の技術】電子部品の焼成炉等においては、壁体か
らの発塵が極力小さいことが望まれる。一方で、焼成炉
の炉壁に用いられる断熱材としては、耐熱性が高く低熱
容量であることから、主としてアルミノシリケート質繊
維を用いてなる耐熱構造体が採用されている。しかし、
アルミノシリケート質繊維を用いた耐熱構造体は、発塵
が比較的多いという問題があり、半導体やディスプレイ
といった電子部品などクリーン性が求められる製造環境
の利用には向いていない。2. Description of the Related Art In a firing furnace for electronic parts, it is desired that dust from the wall is as small as possible. On the other hand, as the heat insulating material used for the furnace wall of the firing furnace, a heat resistant structure mainly made of aluminosilicate fiber is adopted because of its high heat resistance and low heat capacity. But,
The heat-resistant structure using aluminosilicate fiber has a problem that it generates a relatively large amount of dust, and is not suitable for use in a manufacturing environment such as electronic parts such as semiconductors and displays that require cleanliness.
【０００３】[0003]
【発明が解決しようとする課題】そこで、本願の発明者
らは、上記問題を解消するものとして、先に特願２００
０−３８６８９６（特開２００１−２７８６８０）で改
良された耐熱構造体を提案している。前記耐熱構造体と
は、無機繊維質成形体（以下、耐熱基材と呼ぶ）の表面
に、コロイダルシリカ等の無機バインダーに有機バイン
ダー（例えば、ポリエチレンオキサイド）を加えて調製
してなるコーティング剤を塗布し、耐熱被覆層を形成し
た構造体である。Therefore, the inventors of the present application have previously filed a patent application 200 as a solution to the above problems.
0-386896 (JP 2001-278680 A) proposes an improved heat resistant structure. The heat resistant structure is a coating agent prepared by adding an organic binder (for example, polyethylene oxide) to an inorganic binder such as colloidal silica on the surface of an inorganic fibrous molded body (hereinafter referred to as a heat resistant base material). It is a structure coated with a heat resistant coating layer.
【０００４】前記コーティング剤の組成物である無機バ
インダーは、得られる耐熱被覆層にある程度の強度を付
与するために必要なものであり、一方、有機バインダー
は、コーティング剤を塗布し易い粘度に調製するために
必要なものとしている。The inorganic binder, which is a composition of the coating agent, is necessary for imparting a certain degree of strength to the heat-resistant coating layer to be obtained, while the organic binder is prepared to have a viscosity such that the coating agent can be easily applied. It is necessary to do.
【０００５】しかし、上記コーティング剤による耐熱被
覆層を有する耐熱構造体にあっては、炉内の処理温度の
上昇により被覆層に含まれる有機バインダーが揮発して
被加熱製品が汚染されたり、被膜にクラックが生じてし
まうといった不都合が生じることが懸念される。However, in a heat-resistant structure having a heat-resistant coating layer formed of the above coating agent, the organic binder contained in the coating layer is volatilized due to an increase in the treatment temperature in the furnace to contaminate the product to be heated, or the coating film. There is concern that inconvenience may occur such that cracks occur in the.
【０００６】本発明は、上記問題に鑑みてなされたもの
であって、より高い耐熱性を有し、かつ表面からの発塵
を抑制できると共に加熱時に被加熱製品を汚染する有害
物質を発生することのない改良された耐熱構造体を提供
することを目的とする。The present invention has been made in view of the above problems, and has higher heat resistance, can suppress dust generation from the surface, and generates a harmful substance that contaminates a product to be heated during heating. It is an object of the present invention to provide an improved heat-resistant structure that does not have such a problem.
【０００７】[0007]
【課題を解決するための手段】上記目的を達成するた
め、請求項１の発明は、耐熱基材に耐熱被覆層を形成し
てなる耐熱構造体であって、前記耐熱被覆層は、粉末状
耐熱材料６０〜９０重量％と、無機バインダー５〜３０
重量％と、増粘材からなるコーティング剤とで形成され
ていることを要旨とする。In order to achieve the above object, the invention of claim 1 is a heat-resistant structure comprising a heat-resistant coating layer formed on a heat-resistant substrate, wherein the heat-resistant coating layer is in the form of powder. Heat-resistant material 60-90% by weight and inorganic binder 5-30
The gist is that it is formed by a weight percentage and a coating agent made of a thickening material.
【０００８】請求項２の発明は、請求項１に記載の耐熱
構造体において、前記増粘材の含有量は、０．５〜５重
量％であることを要旨とする。A second aspect of the present invention is characterized in that, in the heat-resistant structure according to the first aspect, the content of the thickener is 0.5 to 5% by weight.
【０００９】請求項３の発明は、請求項１または２に記
載の耐熱構造体において、前記増粘材が、平均粒子径５
〜４０ｎｍのフュームドシリカであることを要旨とす
る。According to a third aspect of the present invention, in the heat resistant structure according to the first or second aspect, the thickener has an average particle size of 5
The gist is that it is a fumed silica of -40 nm.
【００１０】請求項４の発明は、請求項１〜３のいずれ
かに記載の耐熱構造体において、前記コーティング剤
は、１〜２０重量％の繊維状耐熱材料をさらに含むこと
を要旨とする。A fourth aspect of the present invention provides the heat resistant structure according to any one of the first to third aspects, wherein the coating agent further contains 1 to 20% by weight of a fibrous heat resistant material.
【００１１】請求項５の発明は、請求項１〜４のいずれ
かに記載の耐熱構造体において、前記耐熱被覆層の表面
には、コロイダルシリカを主材とするコーティング層が
形成されていることを要旨とする。According to a fifth aspect of the present invention, in the heat resistant structure according to any one of the first to fourth aspects, a coating layer containing colloidal silica as a main material is formed on the surface of the heat resistant coating layer. Is the gist.
【００１２】請求項６の発明は、請求項５に記載の耐熱
構造体において、前記コロイダルシリカを主材とするコ
ーティング層は、平均粒子径５０〜６００ｎｍのコロイ
ダルシリカ７０〜９５重量％と、無機バインダー５〜３
０重量％とからなるコーティング剤で形成されることを
要旨とする。According to a sixth aspect of the present invention, in the heat-resistant structure according to the fifth aspect, the coating layer containing the colloidal silica as a main material contains 70 to 95% by weight of colloidal silica having an average particle diameter of 50 to 600 nm and an inorganic material. Binder 5-3
The gist is that it is formed of a coating agent composed of 0% by weight.
【００１３】請求項７の発明は、請求項１〜６のいずれ
かに記載の耐熱構造体において、前記耐熱基材は、無機
質成形体で形成されていることを要旨とする。A seventh aspect of the present invention provides the heat-resistant structure according to any one of the first to sixth aspects, wherein the heat-resistant base material is formed of an inorganic molded body.
【００１４】[0014]
【発明の実施の形態】本発明の好ましい実施の形態とし
ては、耐熱基材に耐熱被覆層を形成してなる耐熱構造体
において、前記耐熱被覆層を、粉末状耐熱材料６０〜９
０重量％と、無機バインダー５〜３０重量％と、増粘材
０．５〜５重量％とからなるコーティング剤で形成す
る。BEST MODE FOR CARRYING OUT THE INVENTION As a preferred embodiment of the present invention, in a heat resistant structure formed by forming a heat resistant coating layer on a heat resistant substrate, the heat resistant coating layer is formed of powdered heat resistant materials 60 to 9
It is formed by a coating agent composed of 0% by weight, an inorganic binder of 5 to 30% by weight, and a thickening agent of 0.5 to 5% by weight.
【００１５】前記耐熱被覆層によれば、耐熱基材に繊維
質成形体が用いられた場合でも、繊維質成形体から発生
する発塵を抑えることができる。According to the heat resistant coating layer, even when a fibrous molded body is used as the heat resistant base material, it is possible to suppress dust generation from the fibrous molded body.
【００１６】前記コーティング剤に用いる耐熱材料とし
ては、アルミナ、ムライト、シリカ、コージェライト、
マグネシア、ジルコニア等の耐熱性のある無機材料から
任意に選択されればよく、２種以上の材料を混合して用
いても良い。耐熱性の観点からは好ましくはアルミナま
たはムライトを使用することが望まれる。As the heat-resistant material used for the coating agent, alumina, mullite, silica, cordierite,
It may be arbitrarily selected from heat-resistant inorganic materials such as magnesia and zirconia, and two or more kinds of materials may be mixed and used. From the viewpoint of heat resistance, it is preferable to use alumina or mullite.
【００１７】また、前記耐熱被覆層の熱膨張係数は、耐
熱基材の熱膨張係数に対して−２５〜＋２５％、好まし
くは−１０〜＋１０％、さらに好ましくは−５〜＋５％
の範囲になるようにすることが好ましい。The coefficient of thermal expansion of the heat resistant coating layer is -25 to + 25%, preferably -10 to + 10%, and more preferably -5 to + 5% with respect to the coefficient of thermal expansion of the heat resistant substrate.
It is preferable to set it in the range.
【００１８】一般的に、接触する２つの材料の熱膨張係
数が異なると、加熱した際、一方の材料の熱膨張が他方
の熱膨張を拘束し、熱応力が発生する。この熱応力が材
料の亀裂や破壊、剥離等の原因となる。Generally, when two materials in contact have different coefficients of thermal expansion, when heated, the thermal expansion of one material restrains the thermal expansion of the other material, resulting in thermal stress. This thermal stress causes cracks, breakage, peeling, etc. of the material.
【００１９】この場合、高温時においても前記耐熱基材
と耐熱被覆層との熱膨張差から生じる亀裂や破壊、剥離
等を防ぐことができ、耐熱性を高めることができる。こ
こで、前記耐熱基材および耐熱被覆層の熱膨張率は、Ｊ
ＩＳ−Ｒ１６１８：ファインセラミックスの熱機械分析
による熱膨張の測定方法に準じた測定方法で測定されれ
ばよく、測定した耐熱基材の熱膨張率をもとに前記コー
ティング剤に用いる耐熱性材料の熱膨張率を考慮して、
その耐熱材料の中から任意に選択して耐熱被覆層の熱膨
張率を調整すればよい。In this case, it is possible to prevent cracks, breakage, peeling and the like caused by the difference in thermal expansion between the heat resistant base material and the heat resistant coating layer even at high temperature, and it is possible to improve heat resistance. Here, the coefficient of thermal expansion of the heat resistant substrate and the heat resistant coating layer is J
IS-R1618: It may be measured by a measuring method according to the measuring method of thermal expansion by thermomechanical analysis of fine ceramics, and based on the measured thermal expansion coefficient of the heat-resistant base material, Considering the coefficient of thermal expansion,
The thermal expansion coefficient of the heat resistant coating layer may be adjusted by arbitrarily selecting from the heat resistant materials.
【００２０】また、コーティング剤に用いる耐熱材料に
は、粉末状耐熱材料のほかに、繊維状耐熱材料が含まれ
ていても良い。この場合、耐熱被覆層の亀裂進展抵抗力
としての靭性が向上し、亀裂を発生させる応力集中を緩
和させることができる。したがって、耐熱被覆層の破壊
には大きなエネルギーが必要となり、その結果、クラッ
クの伝搬を防止することができる。In addition to the powdery heat resistant material, the heat resistant material used for the coating agent may include a fibrous heat resistant material. In this case, the toughness of the heat-resistant coating layer as the crack growth resistance is improved, and the stress concentration causing the cracks can be relaxed. Therefore, a large amount of energy is required to break the heat resistant coating layer, and as a result, the propagation of cracks can be prevented.
【００２１】上記コーティング剤としては、平均粒子径
１〜４０μｍの粉末状耐熱材料６０〜９０重量％と、平
均粒子径１〜５０ｎｍのコロイダルシリカを主成分とす
るバインダー５〜３０重量％と、平均繊維長３０〜２０
０μｍの繊維状耐熱材料１〜２０重量％と、増粘材０．
５〜５重量％とを含有する組成物からなるコーティング
剤が好ましい。As the above coating agent, 60 to 90% by weight of a powdery heat-resistant material having an average particle size of 1 to 40 μm, 5 to 30% by weight of a binder containing colloidal silica having an average particle size of 1 to 50 nm as a main component, and an average of Fiber length 30-20
0 μm of fibrous heat resistant material 1 to 20% by weight, and thickener 0.
A coating agent comprising a composition containing 5 to 5% by weight is preferred.
【００２２】上記コーティング剤は、耐熱基材の表面に
スプレーなどを用いて塗布し、例えば室温で３０分程度
乾燥させたのち、約１０５℃の乾燥機内で１時間以上乾
燥させればよい。こうして耐熱基材の表面には厚さ５０
μｍ〜１ｍｍの耐熱層が形成される。また、コーティン
グ剤の塗布にはハケやヘラ、ローラーなどを使用した公
知の方法で塗布してもよい。The above coating agent may be applied to the surface of the heat-resistant substrate by spraying or the like, dried at room temperature for about 30 minutes, and then dried in a dryer at about 105 ° C. for 1 hour or more. In this way, the thickness of the heat resistant substrate is 50
A heat resistant layer having a thickness of μm to 1 mm is formed. The coating agent may be applied by a known method using a brush, a spatula, a roller or the like.
【００２３】コーティング剤の塗布量としては、耐熱基
材の表面に固形分換算で０．０１〜１ｇ／ｃｍ２の面密
度で塗布することが好ましく、コーティングの耐熱被覆
層の厚さは５０μｍ〜１ｍｍの範囲であることが好まし
い。耐熱被覆層が５０μｍより小さいと強度も弱く低発
塵の効果が得られにくく、１ｍｍを超えると乾燥時のク
ラック発生の原因となるので好ましくない。The coating amount of the coating agent is preferably 0.01-1 g / cm 2 in terms of solid content on the surface of the heat-resistant substrate, and the thickness of the heat-resistant coating layer of the coating is 50 μm- It is preferably in the range of 1 mm. If the heat-resistant coating layer is smaller than 50 μm, the strength is weak and it is difficult to obtain the effect of low dust generation, and if it exceeds 1 mm, cracks are generated during drying, which is not preferable.
【００２４】上記のようにして得られる耐熱被覆層は、
後述する実施例にも示されるように、１２００℃程度ま
での耐熱性に加えて、優れた低発塵性、平滑性を有して
いる。また、製造工程における乾燥時や熱衝撃を受けた
際に亀裂が生じたりすることがない。これは、上述した
ように繊維材による補強対策を行っていることと、耐熱
基材と熱膨張係数を揃えることによって熱応力を緩和し
ているためと推察される。このことは、耐熱被覆層とし
て考えた場合に熱衝撃を受けることで、発塵し易くなっ
たり、剥がれやすくなったりする問題を抑える点で有効
なものとなる。The heat resistant coating layer obtained as described above is
As shown in Examples described later, in addition to heat resistance up to about 1200 ° C., it has excellent low dusting property and smoothness. In addition, cracks do not occur during drying in the manufacturing process or when subjected to thermal shock. It is presumed that this is because the reinforcing measures by the fiber material are taken as described above and the thermal stress is relaxed by making the thermal expansion coefficient the same as that of the heat resistant base material. This is effective in suppressing the problem that dust is likely to be generated and peeling is likely to occur due to thermal shock when considered as a heat resistant coating layer.
【００２５】前記コーティング剤に使用されるコロイダ
ルシリカとしては、市販のもの（粒子径１〜５０ｎｍ）
でよいが、好ましくは、その粒度を調整する必要があ
る。好ましい粒子径の範囲は、一般的に１〜４０ｎｍで
あり、粒子径が１ｎｍ未満であると、バインド力は強い
が脱水縮合時の収縮が大きくなり、マイクロクラックが
発生しやすくなる。一方、粒子径が４０ｎｍを超えると
バインダーとしての強度が弱くなり、発塵しやすくなる
ので好ましくない。特に好ましい粒子径の範囲は１〜３
０ｎｍである。The colloidal silica used in the coating agent is a commercially available product (particle size 1 to 50 nm).
However, it is necessary to adjust the particle size. The preferred particle size range is generally 1 to 40 nm. When the particle size is less than 1 nm, the binding force is strong but the shrinkage during dehydration condensation is large, and microcracks are likely to occur. On the other hand, if the particle size exceeds 40 nm, the strength as a binder becomes weak and dust is easily generated, which is not preferable. Particularly preferred particle size range is 1 to 3.
It is 0 nm.
【００２６】コーティング剤の組成物中のコロイダルシ
リカの割合は５〜３０重量％とされるが、好ましくは、
１０〜２５重量％である。割合が１０重量％未満になる
と、バインダーとしての作用が不十分となり、機械的強
度が低下し十分な接着力が得られない。一方、２５重量
％を超えると一般的に機械的強度が増加するが、耐熱材
料の割合が減少するために耐熱被覆層に亀裂が生じやす
くなり、加えて耐熱被覆層の機械的強度が小さくなると
いう不都合を生じるので好ましくない。The proportion of colloidal silica in the composition of the coating agent is 5 to 30% by weight, preferably
It is 10 to 25% by weight. If the proportion is less than 10% by weight, the action as a binder becomes insufficient, the mechanical strength is lowered, and sufficient adhesive force cannot be obtained. On the other hand, if it exceeds 25% by weight, the mechanical strength generally increases, but since the proportion of the heat-resistant material decreases, cracks easily occur in the heat-resistant coating layer, and in addition, the mechanical strength of the heat-resistant coating layer decreases. This is not preferable because it causes the inconvenience.
【００２７】また、前記コーティング剤に添加される粉
末状耐熱材料としては、アルミナ、ムライト、シリカ、
コージェライト、マグネシア、ジルコニアといった耐熱
性の無機材料を挙げることができる。また、熱膨張係数
を調節するためにこれら２種以上の材料を混合して用い
てもよい。耐熱性の観点からは好ましくはアルミナまた
はムライトを使用することが望まれる。また、熱膨張係
数を調節するために、上記材料から選択されればよい。
前記粉末状耐熱材料の平均粒径は１〜４０μｍとされる
が、好ましくは、１〜３０μｍである。平均粒子径が１
μｍ未満になると、亀裂が発生しやすくなり、３０μｍ
を超えるとコーティングの強度低下、平滑性の低下を引
き起こすので好ましくない。The powdery heat-resistant material added to the coating agent is alumina, mullite, silica,
A heat resistant inorganic material such as cordierite, magnesia or zirconia can be used. Further, these two or more kinds of materials may be mixed and used in order to adjust the thermal expansion coefficient. From the viewpoint of heat resistance, it is preferable to use alumina or mullite. Further, it may be selected from the above materials in order to adjust the coefficient of thermal expansion.
The average particle size of the powdery heat-resistant material is set to 1 to 40 μm, preferably 1 to 30 μm. Average particle size is 1
If it is less than μm, cracks are likely to occur, and 30 μm
When it exceeds, the strength of the coating and the smoothness of the coating are deteriorated, which is not preferable.
【００２８】また、前記粉末状耐熱材料は、平均粒径分
布の異なる大粒径の粉末状耐熱材料と小粒径の粉末状耐
熱材料とを併用することがさらに好ましい。こうした場
合、大粒径の粉末状耐熱材料同士の隙間に小粒径の粉末
状耐熱材料が入り込むことができる。したがって、コー
ティングによる耐熱被覆層において粉末状耐熱材料の充
填密度が高くなり、耐熱被覆層の強度が増す。Further, as the powdery heat-resistant material, it is more preferable to use a powdery heat-resistant material having a large particle diameter and a powdery heat-resistant material having a small particle diameter having different average particle size distributions in combination. In such a case, the powdery heat-resistant material having a small particle size can enter the gap between the powdery heat-resistant materials having a large particle size. Therefore, the packing density of the powdery heat-resistant material is increased in the heat-resistant coating layer formed by coating, and the strength of the heat-resistant coating layer is increased.
【００２９】コーティング剤の組成物中の粉末状耐熱材
料の割合は、一般的に固形分換算で６０〜９０重量％、
好ましくは６５〜８５重量％とされる。粉末状耐熱材料
の割合が６５重量％未満になると相対的に繊維量が減り
クラックが発生しやすくなるという不都合を生じる。一
方、８５重量％を超えると強度が弱くなるので好ましく
ない。The proportion of the powdery heat-resistant material in the composition of the coating agent is generally 60 to 90% by weight in terms of solid content,
It is preferably 65 to 85% by weight. If the proportion of the powdery heat-resistant material is less than 65% by weight, the amount of fibers is relatively reduced and cracks are likely to occur, which is a disadvantage. On the other hand, if it exceeds 85% by weight, the strength becomes weak, which is not preferable.
【００３０】さらに、コーティング剤に添加される繊維
状耐熱材料としては、アルミナ繊維、ムライト繊維、ア
ルミノシリケート繊維といった耐熱性の無機繊維を挙げ
ることができる。これらの材料は、熱膨張係数を調整す
るために任意に選択されればよい。また、これら２種以
上の材料を混合して用いてもよい。さらにまた、これら
の無機繊維においては、無機繊維中のショット含有率が
５重量％以下であることが望ましい。ここで、ショット
とは、無機繊維を製造過程において、繊維とならなかっ
た非繊維のことをいう。ショットは、溶融状態の繊維の
出発材料を飛ばして繊維化する際に飛翔する先端部（こ
の先端部が飛んだ後に尾を引いた部分が繊維となる）が
最終的に残存することで生成される。Further, examples of the fibrous heat-resistant material added to the coating agent include heat-resistant inorganic fibers such as alumina fiber, mullite fiber and aluminosilicate fiber. These materials may be arbitrarily selected to adjust the coefficient of thermal expansion. Further, these two or more materials may be mixed and used. Furthermore, in these inorganic fibers, the shot content in the inorganic fibers is preferably 5% by weight or less. Here, the shot refers to a non-fiber that has not become a fiber in the process of manufacturing an inorganic fiber. The shot is generated by the fact that the tip part that flies when the starting material of the fiber in the molten state is skipped and is made into fiber (the part where the tail is pulled after this tip part has become the fiber) remains finally. It
【００３１】無機繊維材料の平均繊維長を３０〜２００
μｍとするのは、コーティング剤として要求される要求
事項を満足するためである。無機繊維材料は、その存在
によって得られるコーティング層（耐火被覆層）を補強
し、クラックが発生しにくくするものである。しかし、
平均繊維長が３０μｍ以下では補強効果が小さく、目的
とする強度を有したコーティング層が得られない。ま
た、繊維長が２００μｍ以上となると、コート剤を塗布
した際に繊維が凝集あるいは絡み合い、適当な分散性が
得られなくなるので好ましくない。即ち、コート層中で
繊維が凝集しあるいは絡み合い、適当な分散性が得られ
なくなると、コーティング層の材質に局所的な粗密が生
成され、クラックが発生しやすくなるので、そうならな
いようにするために繊維長は２００μｍ以下とすること
が好ましい。The average fiber length of the inorganic fiber material is 30 to 200.
The reason why the thickness is set to μm is to satisfy the requirements required for the coating agent. The inorganic fiber material reinforces the coating layer (fireproof coating layer) obtained by its presence and makes cracks less likely to occur. But,
When the average fiber length is 30 μm or less, the reinforcing effect is small and a coating layer having the desired strength cannot be obtained. Further, if the fiber length is 200 μm or more, the fibers are aggregated or entangled when the coating agent is applied, and appropriate dispersibility cannot be obtained, which is not preferable. That is, when the fibers are aggregated or entangled in the coat layer and proper dispersibility cannot be obtained, local coarseness and denseness are generated in the material of the coating layer, and cracks are easily generated. Further, the fiber length is preferably 200 μm or less.
【００３２】また、無機繊維の配合割合を１〜２０重量
％とするのは、塗布性（塗布のしやすさ）を満足しつ
つ、同時に必要とする補強効果を得るためである。ま
た、コーティング剤中の無機繊維材料は、基材に含まれ
る無機繊維材料と同じ材料とすることが好ましい。こう
することで、基材とコート層の熱膨張率あるいは熱的な
性質を近づけることができ、クラックの発生やコート層
の剥離の問題をさらに抑制できる。The content of the inorganic fiber is set to 1 to 20% by weight in order to satisfy the coating property (easiness of coating) and at the same time obtain the required reinforcing effect. The inorganic fiber material in the coating agent is preferably the same as the inorganic fiber material contained in the base material. By doing so, the coefficient of thermal expansion or the thermal properties of the base material and the coat layer can be made close to each other, and the problems of cracking and peeling of the coat layer can be further suppressed.
【００３３】コーティング剤に添加される増粘材として
は、例えば、ベントナイトやスメクタイトといった粘土
が使用されてもよい。As the thickening agent added to the coating agent, for example, clay such as bentonite or smectite may be used.
【００３４】増粘材は、コーティング層を塗布しやす
く、また必要とする物性を有するコーティング層（耐火
被覆層）を得るために重要な役割を果たす。増粘材は
０．５〜５重量％とすることで、良好な塗布性に必要と
されるコーティング剤の伸び（良好な塗布性）が得ら
れ、またコーティング層を形成する際に必要な保水性が
得られる。保水性が適当でないと、コーティング剤を塗
布した際にコロイダルシリカ等の無機バインダーが耐熱
基材にしみ込み過ぎ、コーティング層を保持するのに必
要なバインド効果が得られなくなる。また、無機バイン
ダーが基材にしみ込むことで無機粒子が表面に浮いた存
在となり、期待に反して無機粒子が飛散しやすい状態と
なってしまう。即ち、かえって粉っぽいものとなってし
まう。また、保水性を適当なものとすることで、無機バ
インダーが適度に基材にしみこみ、耐熱基材とコーティ
ング層との結合力を高くし、コーティング層が耐熱基材
から剥離しにくいものが得られる。増粘材の配合量を上
記範囲とすることで、上述した適当な保水性を有したコ
ーティング剤を得ることができる。The thickening agent plays an important role in easily applying the coating layer and obtaining a coating layer (fireproof coating layer) having the required physical properties. By adjusting the content of the thickening agent to 0.5 to 5% by weight, the elongation of the coating agent required for good coatability (good coatability) can be obtained, and the water retention necessary for forming the coating layer can be obtained. Sex is obtained. If the water retention is not appropriate, the inorganic binder such as colloidal silica will soak into the heat-resistant substrate too much when the coating agent is applied, and the binding effect necessary for holding the coating layer cannot be obtained. In addition, the inorganic binder floats on the surface due to the inorganic binder penetrating the base material, and the inorganic particles are likely to scatter unexpectedly. That is, it becomes powdery. In addition, by setting the water retention property to an appropriate value, the inorganic binder permeates the base material appropriately, increasing the bond strength between the heat resistant base material and the coating layer, and the coating layer is difficult to peel from the heat resistant base material. To be By setting the compounding amount of the thickener within the above range, the coating agent having the appropriate water retention described above can be obtained.
【００３５】前記増粘材には平均粒子径１００ｎｍ未満
のアルミナ、ムライト、シリカ、コージェライト、マグ
ネシア、ジルコニアといった耐熱性の無機材料からなる
微粉末状耐熱材料が含有されることが好ましい。さら
に、このような微粉末状耐熱材料としては、フュームド
シリカがより好ましい。The thickening agent preferably contains a fine powder heat-resistant material made of a heat-resistant inorganic material such as alumina, mullite, silica, cordierite, magnesia and zirconia having an average particle diameter of less than 100 nm. Further, fumed silica is more preferable as such a fine powdery heat-resistant material.
【００３６】ここで、フュームドシリカ（Fumed Silic
a）とは、酸水素炎中に揮発性シラン化合物、主として
四塩化珪素をガス状態で導入し高温下で加水分解するこ
とにより得られる平均粒径５〜４０ｎｍの超微粉末状の
シリカをいう。このフュームドシリカによれば、個々の
フュームドシリカ粒子の表面にあるシラノール基が水素
結合して三次元網目構造を形成するため、液体に少量添
加することにより、その流動性を大きく改善することが
できる。その結果、有機物を用いずに組成物の粘度を高
めることができる。こうした場合、有機物を添加するこ
となくコーティング剤を製造することができるので、加
熱時に発煙や臭いを発する問題もなく、使用時において
も被加熱製品が汚染されることがなくなる。Here, the fumed silica (Fumed Silic
a) refers to ultrafine powdery silica having an average particle size of 5 to 40 nm obtained by introducing a volatile silane compound, mainly silicon tetrachloride, in a gas state into an oxyhydrogen flame and hydrolyzing it at a high temperature. . According to this fumed silica, the silanol groups on the surface of each fumed silica particle are hydrogen-bonded to form a three-dimensional network structure. Therefore, by adding a small amount to a liquid, its fluidity can be greatly improved. You can As a result, the viscosity of the composition can be increased without using an organic substance. In such a case, since the coating agent can be produced without adding an organic substance, there is no problem of producing smoke or odor during heating, and the product to be heated is not contaminated during use.
【００３７】増粘材に含有される微粉末状耐熱材料の平
均粒子径は５〜４０ｎｍ、好ましくは５〜３０ｎｍであ
る。微粉末状耐熱材料の平均粒子径が５ｎｍより小さい
と増粘性が強すぎ、４０ｎｍを超えると微粉末状耐熱材
料の比表面積が小さくなり増粘性が弱くなり好ましくは
ない。The fine powdery heat-resistant material contained in the thickener has an average particle size of 5 to 40 nm, preferably 5 to 30 nm. If the average particle size of the fine powdery heat-resistant material is less than 5 nm, the viscosity increase becomes too strong, and if it exceeds 40 nm, the specific surface area of the fine powdery heat-resistant material becomes small and the viscosity increase becomes weak, which is not preferable.
【００３８】さらに、コーティング剤組成物は、水の添
加により任意の粘度とすることができ、１〜５０００ｃ
Ｐの範囲が好ましい。組成物中の水分量は、固形分合計
１００重量部に対して、５０〜１５０重量部であること
が好ましく、８０〜１００重量部であることがさらに好
ましい。Further, the coating agent composition can be made to have an arbitrary viscosity by adding water, and the coating composition has a viscosity of 1 to 5000 c.
A range of P is preferred. The amount of water in the composition is preferably 50 to 150 parts by weight, and more preferably 80 to 100 parts by weight, based on 100 parts by weight of the total solid content.
【００３９】また、本発明の耐熱構造体は、前記コーテ
ィング剤の耐熱被覆層の表面に、その耐熱被覆層と組成
の異なるコーティング剤による耐熱被覆層（以下、平滑
層と呼称する）が形成されていてもよい。Further, in the heat resistant structure of the present invention, a heat resistant coating layer (hereinafter referred to as a smooth layer) made of a coating agent having a composition different from that of the heat resistant coating layer is formed on the surface of the heat resistant coating layer of the coating agent. May be.
【００４０】ここで、前記平滑層の組成とは、後述する
耐熱材料の種類や配合割合の違いだけでなく、使用され
る耐熱材料の粒径の違いを含む。例えば、このような違
いは顕微鏡などを使用して前記耐熱被覆層と平滑層の境
目を目視で確認できれば良い。Here, the composition of the smooth layer includes not only the difference in the kind and blending ratio of the heat-resistant material described later, but also the difference in particle size of the heat-resistant material used. For example, such a difference may be obtained by visually confirming the boundary between the heat resistant coating layer and the smooth layer using a microscope or the like.
【００４１】上記平滑層を実現するために、例えば、平
均粒子径５０〜６００ｎｍのコロイダルシリカ７０〜９
５重量％と、平均粒子径１〜５０ｎｍのコロイダルシリ
カ５〜３０重量％とを含有する組成物からなるコーティ
ング剤が提供されればよい。In order to realize the above smooth layer, for example, colloidal silica 70 to 9 having an average particle diameter of 50 to 600 nm is used.
It suffices to provide a coating agent composed of a composition containing 5% by weight and 5 to 30% by weight of colloidal silica having an average particle size of 1 to 50 nm.
【００４２】上記コーティング剤は、前記耐熱被覆層の
表面にスプレーなどを用いて塗布され、例えば室温で３
０分程度乾燥させたのち、約１０５℃の乾燥機内で１時
間以上乾燥させればよい。こうして耐熱基材の表面また
は前記耐熱被覆層の表面には厚さ５〜１００μｍの平滑
層が形成される。また、コーティング剤の塗布にはハケ
やローラーのようなもので塗布されてもよい。The coating agent is applied to the surface of the heat resistant coating layer by using a spray or the like, and is applied at room temperature, for example.
After drying for about 0 minutes, it may be dried in a dryer at about 105 ° C. for 1 hour or more. Thus, a smooth layer having a thickness of 5 to 100 μm is formed on the surface of the heat resistant substrate or the surface of the heat resistant coating layer. The coating agent may be applied with a brush or a roller.
【００４３】このようにして得られる平滑層は、後述さ
れる実施例にも示すように、１２００℃程度までの耐熱
性に加えて、優れた低発塵性、平滑性を有している。ま
た、製造工程における乾燥時や熱衝撃を受けた際に亀裂
が生じたりすることがない。これは、平滑層に用いる粒
子が微細であることと同時にミクロンオーダーでの多孔
性を持っているため、耐熱衝撃性が良好であるとともに
剥離や発塵を防止できるためと推察される。このこと
は、平滑層として考えた場合に熱衝撃を受けることで、
発塵し易くなったり、剥がれやすくなったりする問題を
抑える点で有効なものとなる。The smooth layer thus obtained has, in addition to heat resistance up to about 1200 ° C., excellent low dusting property and smoothness, as will be shown in Examples described later. In addition, cracks do not occur during drying in the manufacturing process or when subjected to thermal shock. It is speculated that this is because the particles used for the smooth layer are fine and at the same time have porosity on the order of microns, so that they have good thermal shock resistance and can prevent peeling and dust generation. This is because when it is considered as a smooth layer, it is subjected to thermal shock,
This is effective in suppressing the problems that dust is easily generated and peeling is easily caused.
【００４４】平滑層コーティング剤の塗布量としては、
前記耐熱基材の表面に固形分換算で０．００３〜０．０
５ｇ／ｃｍ２の面密度で塗布することが好ましく、層の
厚さは５〜１００μｍの範囲であることが好ましい。５
μｍ未満であると十分な平滑性が得られず、１００μｍ
を超えると乾燥時の割れ等を引き起こすので好ましくな
い。The coating amount of the smoothing layer coating agent is
0.003 to 0.0 in terms of solid content on the surface of the heat resistant substrate
It is preferable to apply it at an areal density of 5 g / cm 2 , and the thickness of the layer is preferably in the range of 5 to 100 μm. 5
If it is less than μm, sufficient smoothness cannot be obtained, and 100 μm
If it exceeds the range, cracks and the like may occur during drying, which is not preferable.
【００４５】前記組成物に使用されるコロイダルシリカ
としては、市販のもの（平均粒子径１〜５０ｎｍ）でよ
いが、好ましくは、その粒度を調整する必要がある。好
ましい平均粒子径の範囲は、一般的に１〜４０ｎｍであ
り、粒子径が１ｎｍ未満であると、バインド力は強いが
脱水縮合時の収縮が大きくなり、マイクロクラックが発
生しやすくなる。一方、粒子径が４０ｎｍを超えるとバ
インダーとしての強度が弱くなるため、発塵しやすくな
るので好ましくない。特に好ましい粒子径の範囲は１〜
３０ｎｍである。The colloidal silica used in the composition may be a commercially available one (average particle size 1 to 50 nm), but it is preferable to adjust the particle size. The preferable range of the average particle diameter is generally 1 to 40 nm. When the particle diameter is less than 1 nm, the binding force is strong but the shrinkage during dehydration condensation is large, and microcracks are likely to occur. On the other hand, if the particle size exceeds 40 nm, the strength as a binder becomes weak and dust is easily generated, which is not preferable. Particularly preferred particle size range is 1 to
It is 30 nm.
【００４６】平滑層を形成するコーティング剤組成物中
の平均粒子径１〜５０ｎｍのコロイダルシリカの割合
は、５〜３０重量％とされるが、好ましくは、１０〜２
５重量％である。割合が１０重量％未満になると、バイ
ンダーとしての作用が不十分となり、機械的強度が低下
し十分な接着力が得られない。一方、２５重量％を超す
と一般的に機械的強度が増加するが、耐熱材料としての
割合が減少するために平滑層に亀裂が生じやすくなり、
加えて平滑層の機械的強度が小さくなるという不都合を
生じるので好ましくない。The proportion of colloidal silica having an average particle size of 1 to 50 nm in the coating agent composition for forming a smooth layer is 5 to 30% by weight, preferably 10 to 2%.
It is 5% by weight. If the proportion is less than 10% by weight, the action as a binder becomes insufficient, the mechanical strength is lowered, and sufficient adhesive force cannot be obtained. On the other hand, if it exceeds 25% by weight, mechanical strength generally increases, but since the proportion as a heat-resistant material decreases, cracking is likely to occur in the smooth layer,
In addition, the mechanical strength of the smooth layer is reduced, which is not preferable.
【００４７】また、前記平滑層を形成するコーティング
剤組成物に使用されるコロイダルシリカには平均径５〜
２０ｎｍ、平均長４０〜３００ｎｍの細長い形状をした
ものが使用されてもよい。このような形状のコロイダル
シリカによれば、粒状のコロイダルシリカと比べて、周
囲の粒子との絡みつきが良くなり、耐熱基材への浸透が
防止されて良好な被膜性を得ることができる。また、容
易に増粘性を高めることができ、溶媒としての水が耐熱
基材へ浸透することを防止できる。その結果、粒子間の
バインド力が強くなり平滑層の表面は良好な平滑性が得
られる。The colloidal silica used in the coating composition for forming the smooth layer has an average diameter of 5 to 5.
An elongated shape having a thickness of 20 nm and an average length of 40 to 300 nm may be used. According to the colloidal silica having such a shape, as compared with the granular colloidal silica, the entanglement with surrounding particles is improved, the permeation into the heat-resistant base material is prevented, and good coatability can be obtained. Further, the thickening property can be easily increased, and water as a solvent can be prevented from penetrating into the heat resistant base material. As a result, the binding force between particles becomes strong, and the surface of the smooth layer has good smoothness.
【００４８】また、平滑層を形成するコーティング剤組
成物中には、平均粒径０．１〜５μｍの粉末状耐熱材料
が１〜３０重量％含有されていてもよい。この粉末状耐
熱材料によれば、例えば、加熱時に脱水縮合によってコ
ロイダルシリカが収縮した場合でも、粉末状耐熱材料が
わずかに熱膨張することによってコロイダルシリカの収
縮量を埋め合わせをすることができる。その結果、高温
時に発生する微細なクラックの発生を防止することがで
きる。Further, the coating composition for forming the smooth layer may contain 1 to 30% by weight of a powdery heat-resistant material having an average particle size of 0.1 to 5 μm. According to this powdery heat-resistant material, for example, even if the colloidal silica shrinks due to dehydration condensation during heating, the powdery heat-resistant material is slightly thermally expanded to compensate for the shrinkage of the colloidal silica. As a result, it is possible to prevent the generation of fine cracks that occur at high temperatures.
【００４９】前記コーティング剤組成物中に添加される
耐熱材料としては、アルミナ、ムライト、シリカ、コー
ジェライト、マグネシア、ジルコニアといった耐熱性の
無機材料を挙げることができる。また、これら２種以上
の材料を混合して用いてもよい。Examples of the heat resistant material added to the coating agent composition include heat resistant inorganic materials such as alumina, mullite, silica, cordierite, magnesia and zirconia. Further, these two or more materials may be mixed and used.
【００５０】さらに、上記組成物は水の添加により任意
の粘度とすることができ、１〜５０００ｃＰの範囲が好
ましい。組成物中の水分量は、固形分合計１００重量部
に対して、１００〜３００重量部であることが好まし
く、１５０〜２５０重量部であることがより好ましい。Further, the above composition can be made to have an arbitrary viscosity by adding water, and the range of 1 to 5000 cP is preferable. The amount of water in the composition is preferably 100 to 300 parts by weight, and more preferably 150 to 250 parts by weight, based on 100 parts by weight of the total solid content.
【００５１】本発明に係る前記耐熱被覆層および平滑層
を形成するコーティング剤を製造する際に、バインダー
と耐熱性材料およびその他の補助剤の混合方法としては
公知の方法を用いることができ、通常、羽根撹拌、ライ
カイ器などによる混合、ボールミルなどによる混合など
が使用できる。In producing the coating agent for forming the heat-resistant coating layer and the smooth layer according to the present invention, a known method can be used as a method for mixing the binder with the heat-resistant material and other auxiliary agents, , Blade stirring, mixing with a liquor, mixing with a ball mill, etc. can be used.
【００５２】本発明において、前記耐熱被覆層が形成さ
れる耐熱基材としては、例えば、アルミナ繊維やアルミ
ノシリケート繊維といった耐熱性繊維の成形体からなる
繊維質断熱材や、耐熱性材料からなる多孔質成形断熱
材、ケイ酸カルシウム質成形断熱材などの公知の断熱材
などが適当であり、耐熱性をはじめとして、上述した諸
特性を付与することができる。特に高温域での耐熱性お
よび低発塵性を備えていることから電子部品の焼成炉な
どで用いられる断熱材として好適である。In the present invention, the heat-resistant base material on which the heat-resistant coating layer is formed is, for example, a fibrous heat insulating material formed of a molded product of heat resistant fiber such as alumina fiber or aluminosilicate fiber, or a porous material formed of heat resistant material. Well-known heat insulating materials such as quality molded heat insulating materials and calcium silicate quality heat insulating materials are suitable, and the above-mentioned various properties such as heat resistance can be imparted. In particular, since it has heat resistance in a high temperature range and low dust generation, it is suitable as a heat insulating material used in a firing furnace for electronic parts.
【００５３】[0053]
【実施例】以下に本発明の実施例および比較例を挙げて
具体的に説明する。
実施例１
水８５重量部に対しバインダーとしてのコロイダルシリ
カ（平均粒径２０ｎｍ）１３重量部と、粉末状耐熱性材
料としての平均粒径７μｍのムライト粉末５０重量部
と、同じく粉末状耐熱性材料としての平均粒径２μｍの
ムライト粉末２７重量部と、繊維状耐熱材料としてのア
ルミノシリケート繊維（平均繊維長５０μｍ、平均繊維
径２μｍ）８重量部と、増粘材としてのフュームドシリ
カ（平均粒径１０ｎｍ）２重量部とを混合し、良く撹拌
して耐熱被覆層用のコーティング剤を得た。EXAMPLES The present invention will be specifically described below with reference to Examples and Comparative Examples. Example 1 13 parts by weight of colloidal silica (average particle size 20 nm) as a binder to 85 parts by weight of water, 50 parts by weight of mullite powder having an average particle size of 7 μm as a powdery heat resistant material, and the same powdery heat resistant material 27 parts by weight of mullite powder having an average particle size of 2 μm, 8 parts by weight of aluminosilicate fiber (average fiber length 50 μm, average fiber diameter 2 μm) as a fibrous heat-resistant material, and fumed silica (average particle size) 2 parts by weight (diameter 10 nm) and mixed well to obtain a coating agent for the heat resistant coating layer.
【００５４】耐熱基材としては、アルミノシリケート繊
維１００重量部、コロイダルシリカ８重量部、有機バイ
ンダー（ポリアクリルアミド）１重量部を混合調製した
スラリーから吸引脱水成形法により厚さ５０ｍｍ、幅３
００ｍｍ、長さ３００ｍｍの成形体を形成し、それを乾
燥させて密度０．２５ｇ／ｃｍ３、熱膨張係数４．１×
１０−６／℃のアルミノシリケート繊維質断熱材を得
た。As the heat-resistant base material, a slurry prepared by mixing 100 parts by weight of aluminosilicate fiber, 8 parts by weight of colloidal silica and 1 part by weight of an organic binder (polyacrylamide) by a suction dehydration molding method has a thickness of 50 mm and a width of 3 mm.
A molded body having a length of 00 mm and a length of 300 mm is formed and dried to have a density of 0.25 g / cm 3 and a thermal expansion coefficient of 4.1 ×.
An aluminosilicate fibrous heat insulating material of 10 −6 / ° C. was obtained.
【００５５】次に、前記耐熱基材としてのアルミノシリ
ケート繊維質断熱材の表面に、前記コーティング剤を固
形分換算で０．０４５ｇ／ｃｍ２の面密度でスプレーで
塗布し、室温で３０分乾燥させた後、約１０５℃の乾燥
機で１時間以上乾燥させ、厚さ５００μｍ、熱膨張係数
４．０×１０−６／℃の耐熱被覆層が耐熱基材上に形成
された耐熱構造体を得た。Next, the coating agent was sprayed onto the surface of the aluminosilicate fibrous heat insulating material as the heat-resistant base material at an area density of 0.045 g / cm 2 in terms of solid content, and dried at room temperature for 30 minutes. After that, it is dried in a drier at about 105 ° C. for 1 hour or more to obtain a heat resistant structure having a heat resistant coating layer having a thickness of 500 μm and a thermal expansion coefficient of 4.0 × 10 −6 / ° C. formed on the heat resistant substrate. Obtained.
【００５６】実施例２
水１８０重量部に対しバインダーとして平均粒径５ｎｍ
の球状のコロイダルシリカ６重量部と、同じくバインダ
ーとして平均粒径１０ｎｍ、平均長１００ｎｍの細長い
形状のコロイダルシリカ６重量部と、耐熱材料としての
コロイダルシリカ（平均粒径５００ｎｍ）８８重量部と
を混合し、良く撹拌して平滑層用のコーティング剤を得
た。Example 2 180 parts by weight of water used as a binder had an average particle size of 5 nm.
6 parts by weight of spherical colloidal silica, 6 parts by weight of elongated colloidal silica having an average particle size of 10 nm and an average length of 100 nm as a binder, and 88 parts by weight of colloidal silica (average particle size of 500 nm) as a heat-resistant material are mixed. Then, the mixture was stirred well to obtain a coating agent for a smooth layer.
【００５７】実施例１で得た耐熱構造体（アルミノシリ
ケート繊維質断熱材の耐熱基材の表面に耐熱被覆層が形
成された）の表面に前記平滑層用コーティング剤を固形
分換算で０．００６ｇ／ｃｍ２の面密度で塗布し、室温
で３０分乾燥させた後、約１０５℃の乾燥機で１時間以
上乾燥させ、前記耐熱被覆層の表面に厚さ約３０μｍの
平滑層が形成された耐熱構造体を得た。On the surface of the heat-resistant structure obtained in Example 1 (the heat-resistant coating layer was formed on the surface of the heat-resistant base material of the aluminosilicate fibrous heat insulating material), the smoothing layer coating agent was added in an amount of 0. The coating was applied at an areal density of 006 g / cm 2 , dried at room temperature for 30 minutes, and then dried for 1 hour or more in a dryer at about 105 ° C. to form a smooth layer having a thickness of about 30 μm on the surface of the heat resistant coating layer. A heat resistant structure was obtained.
【００５８】実施例３
水８５重量部に対しバインダーとしてのコロイダルシリ
カ（平均粒径２０ｎｍ）１３重量部と、粉末状耐熱性材
料としての平均粒径５μｍのアルミナ粉末７７重量部
と、繊維状耐熱材料としてのアルミノシリケート繊維
（平均繊維長５０μｍ、平均繊維径２μｍ）８重量部
と、増粘材としてのフュームドシリカ（平均粒径１０ｎ
ｍ）２重量部とを混合し、良く撹拌して耐熱被覆層用の
コーティング剤を得た。Example 3 13 parts by weight of colloidal silica (average particle size 20 nm) as a binder, 85 parts by weight of water, 77 parts by weight of alumina powder having an average particle size of 5 μm as a powdery heat resistant material, and a fibrous heat resistant material 8 parts by weight of aluminosilicate fiber (average fiber length 50 μm, average fiber diameter 2 μm) as material, and fumed silica (average particle size 10 n
m) 2 parts by weight were mixed and stirred well to obtain a coating agent for the heat resistant coating layer.
【００５９】耐熱基材としては、アルミナ繊維３０重量
部、アルミナ粒子７０重量部、コロイダルシリカ８重量
部、有機バインダー（ポリアクリルアミド）１重量部を
混合調製したスラリーから吸引脱水成形法により厚さ５
０ｍｍ、幅３００ｍｍ、長さ３００ｍｍの成形体を形成
し、それを乾燥させて密度０．７０ｇ／ｃｍ３、熱膨張
係数６．０×１０−６／℃のアルミナ繊維質断熱材を得
た。As the heat-resistant substrate, 30 parts by weight of alumina fiber, 70 parts by weight of alumina particles, 8 parts by weight of colloidal silica, and 1 part by weight of organic binder (polyacrylamide) were mixed and prepared, and a thickness of 5 was obtained by a suction dehydration molding method.
A molded body having a size of 0 mm, a width of 300 mm and a length of 300 mm was formed and dried to obtain an alumina fibrous heat insulating material having a density of 0.70 g / cm 3 and a thermal expansion coefficient of 6.0 × 10 −6 / ° C.
【００６０】次に、前記耐熱基材としてのアルミナ繊維
質断熱材の表面に、前記コーティング剤を固形分換算で
０．０４５ｇ／ｃｍ２の面密度でスプレー塗布し、室温
で３０分乾燥させた後、約１０５℃の乾燥機で１時間以
上乾燥させ、アルミナ繊維質断熱材の表面に厚さ約６０
０μｍ、熱膨張係数６．２×１０−６／℃の耐熱被覆層
を形成し、さらに、この耐熱被覆層の表面に実施例２で
得た平滑用コーティング剤を固形分換算で０．００６ｇ
／ｃｍ２の面密度で塗布し、室温で３０分乾燥させた
後、約１０５℃の乾燥機で１時間以上乾燥させ、耐熱層
の表面に厚さ約３０μｍの平滑層が形成された耐熱構造
体を得た。Next, the coating agent was spray-applied to the surface of the alumina fibrous heat insulating material as the heat-resistant substrate at a surface density of 0.045 g / cm 2 in terms of solid content, and dried at room temperature for 30 minutes. Then, it is dried in a dryer at about 105 ° C for 1 hour or more, and the thickness of the alumina fibrous heat insulating material is about 60
A heat-resistant coating layer having a thickness of 0 μm and a thermal expansion coefficient of 6.2 × 10 −6 / ° C. was formed, and 0.006 g of the smoothing coating agent obtained in Example 2 was calculated on the surface of the heat-resistant coating layer in terms of solid content.
Heat-resistant structure in which a smooth layer with a thickness of about 30 μm is formed on the surface of the heat-resistant layer after being applied at an area density of / cm 2 and dried at room temperature for 30 minutes and then dried in a dryer at about 105 ° C. for 1 hour or more. Got the body
【００６１】実施例４
耐熱基材として、生石灰３０重量部、珪石３０重量部、
ワラストナイト３３重量部、シリカ２重量部、カーボン
ファイバー５重量部を混合調製したスラリーから脱水プ
レス成形法により厚さ５０ｍｍ、幅３００ｍｍ、長さ３
００ｍｍの成形体を形成し、オートクレーブにて養生し
て、それを乾燥させて密度が０．８０ｇ／ｃｍ３、熱膨
張係数６．５×１０−６／℃のケイ酸カルシウム質断熱
材を得た。Example 4 As a heat-resistant base material, 30 parts by weight of quick lime, 30 parts by weight of silica stone,
From a slurry prepared by mixing and mixing 33 parts by weight of wollastonite, 2 parts by weight of silica, and 5 parts by weight of carbon fiber, by a dehydration press molding method, a thickness of 50 mm, a width of 300 mm, and a length of 3
A molded body of 00 mm is formed, cured in an autoclave, and dried to obtain a calcium silicate heat insulating material having a density of 0.80 g / cm 3 and a thermal expansion coefficient of 6.5 × 10 −6 / ° C. It was
【００６２】次に前記耐熱基材としてのケイ酸カルシウ
ム質断熱材の表面に、実施例３の耐熱被覆層用のコーテ
ィング剤を固形分換算で０．０４５ｇ／ｃｍ２の面密度
でスプレー塗布し、室温で３０分乾燥させた後、約１０
５℃の乾燥機で１時間以上乾燥させ、基材表面に厚さ６
００μｍ、熱膨張係数６．２×１０−６／℃の耐熱被覆
層を形成し、さらに実施例２の平滑層用のコーティング
剤を固形分換算で０．０１０ｇ／ｃｍ２の面密度でスプ
レーで塗布し、室温で３０分乾燥させた後、約１０５℃
の乾燥機で１時間以上乾燥させ、ケイ酸カルシウム質断
熱材の表面に厚さ約５０μｍの平滑層が形成された耐熱
構造体を得た。Next, the coating agent for the heat-resistant coating layer of Example 3 was spray-coated at a surface density of 0.045 g / cm 2 in terms of solid content on the surface of the calcium silicate heat insulating material as the heat-resistant substrate. After drying at room temperature for 30 minutes, about 10
Dry for 1 hour or more in a dryer at 5 ° C to give a thickness of 6
A heat-resistant coating layer having a thickness of 00 μm and a thermal expansion coefficient of 6.2 × 10 −6 / ° C. was formed, and the coating agent for a smooth layer of Example 2 was sprayed at a surface density of 0.010 g / cm 2 in terms of solid content. After coating and drying at room temperature for 30 minutes, about 105 ℃
Was dried for 1 hour or more by a drier to obtain a heat-resistant structure in which a smooth layer having a thickness of about 50 μm was formed on the surface of the calcium silicate heat insulating material.
【００６３】比較例１
実施例１で用いた耐熱基材であるアルミノシリケート繊
維質断熱材（熱膨張係数４．０×１０−６／℃）の表面
に、水８５重量部に対しバインダーとして平均粒径２０
μｍのコロイダルシリカ１３重量部と、平均粒径７μｍ
のムライト粉末５０重量部と、平均粒径２μｍのムライ
ト粉末２７重量部と、平均繊維長５０μｍ、平均繊維径
２μｍのアルミノシリケート繊維８重量部と、ポリエチ
レンオキサイド０．６重量部と、メチルセルロース１．
４重量部とを混合して得たコーティング剤を固形分換算
で０．０４５ｇ／ｃｍ２の面密度でスプレーで塗布し、
室温で３０分乾燥させた後、約１０５℃の乾燥機で１時
間以上乾燥させ、アルミノシリケート繊維質断熱材の表
面に、厚さ約６００μｍ、熱膨張係数４．０×１０ −６
／℃の耐熱被覆層が形成し、さらにその表面に、実施例
２の平滑用コーティング剤を固形分換算で０．０１０ｇ
／ｃｍ２の面密度でスプレー塗布し、室温で３０分乾燥
させた後、約１０５℃の乾燥機で１時間以上乾燥させ、
厚さ約５０μｍの平滑層が形成された耐熱構造体を得
た。Comparative Example 1
Aluminosilicate fiber which is the heat-resistant substrate used in Example 1
Fiber insulation (coefficient of thermal expansion 4.0 × 10-6/ ° C) surface
The average particle size of 20 as a binder for 85 parts by weight of water
13 parts by weight of colloidal silica of μm and average particle size of 7 μm
Mullite powder of 50 parts by weight and an average particle size of 2 μm
27 parts by weight of powder, average fiber length 50 μm, average fiber diameter
8 parts by weight of 2 μm aluminosilicate fiber and polyethylene
0.6 parts by weight lenoxide and 1.
The coating agent obtained by mixing with 4 parts by weight is converted into solid content.
0.045 g / cmTwoApply by spraying with an areal density of
After drying at room temperature for 30 minutes, use a dryer at about 105 ° C for 1:00
Allow to dry for longer than a period, and then apply aluminosilicate fiber insulation
Thickness is about 600μm, thermal expansion coefficient is 4.0 × 10 -6
/ ° C heat-resistant coating layer is formed,
0.010 g of 2 smoothing coating agent in terms of solid content
/ CmTwoSpray coating at surface density of 30 minutes and dry at room temperature for 30 minutes
After drying, dry in a dryer at about 105 ° C for 1 hour or more,
A heat-resistant structure having a smooth layer with a thickness of about 50 μm is obtained.
It was
【００６４】比較例２
実施例３で用いた耐熱基材であるアルミナ繊維質断熱材
（熱膨張係数６．０×１０−６／℃）の表面に、比較例
１で用いた耐熱被覆層のコーティング剤を固形分換算で
０．０４５ｇ／ｃｍ２の面密度でスプレーで塗布し、室
温で３０分乾燥させた後、約１０５℃の乾燥機で１時間
以上乾燥させ、アルミナ繊維質断熱材の表面に、厚さ約
６００μｍ、熱膨張係数４．０×１０−６／℃の耐熱被
覆層を形成し、さらにこの耐熱被覆層の表面に比較例１
で得た平滑層用のコーティング剤を固形分換算で０．０
０６ｇ／ｃｍ２の面密度で塗布し、室温で３０分乾燥さ
せた後、約１０５℃の乾燥機で１時間以上乾燥させ、耐
熱被覆層の表面に厚さ約３０μｍの平滑層が形成された
耐熱構造体を得た。上記各実施例および比較例で得られ
た耐熱構造体について、熱衝撃性および発塵性、平滑性
を評価した。Comparative Example 2 The heat-resistant coating layer used in Comparative Example 1 was formed on the surface of the alumina fibrous heat insulating material (coefficient of thermal expansion 6.0 × 10 −6 / ° C.) which is the heat-resistant substrate used in Example 3. The coating agent is applied by spraying at an area density of 0.045 g / cm 2 in terms of solid content, dried at room temperature for 30 minutes, and then dried in a dryer at about 105 ° C. for 1 hour or more to obtain an alumina fibrous heat insulating material. A heat-resistant coating layer having a thickness of about 600 μm and a thermal expansion coefficient of 4.0 × 10 −6 / ° C. was formed on the surface, and Comparative Example 1 was formed on the surface of the heat-resistant coating layer.
The coating agent for the smooth layer obtained in step 1 was converted to a solid content of 0.0
The coating was applied at an areal density of 06 g / cm 2 , dried at room temperature for 30 minutes, and then dried at about 105 ° C. for 1 hour or more to form a smooth layer having a thickness of about 30 μm on the surface of the heat resistant coating layer. A heat resistant structure was obtained. The thermal shock resistance, dust generation, and smoothness of the heat resistant structures obtained in each of the above Examples and Comparative Examples were evaluated.
【００６５】ここで、熱衝撃性の評価は、１２００℃に
保持された電気炉に耐熱構造体を投入し、３０分保持し
た後に炉から取り出し、それを強制空冷により冷却した
後に被覆表面の状態を目視により観察し、亀裂などの発
生のないものを「○」、亀裂などが発生しているが致命
的でないものを「△」、使用に耐えないレベルの亀裂等
が発生しているものを「×」、として評価した。Here, the thermal shock resistance was evaluated by placing the heat-resistant structure in an electric furnace maintained at 1200 ° C., holding it for 30 minutes, taking it out of the furnace, cooling it by forced air cooling, and then measuring the state of the coated surface. By visually observing, those with no cracks etc. are marked with "○", those with cracks etc. that are not fatal are marked with "△", those with cracks at a level that cannot withstand use, etc. It was evaluated as "x".
【００６６】また、発塵性の評価は、下記のような方法
で得られる発塵指数で評価した。
サンプル（耐熱構造体）の上面からサンプルの表面に
圧力３×１０４Ｎ／ｍ２で「ニチバン製セロテープ；Ｃ
Ｔ−２４ 幅２４ｍｍ」を貼り付ける。
５秒の静置後、サンプルから粘着テープを剥がす。
剥がした粘着テープを黒色紙上に貼り付け、明度指数
を測定する。
次式により発塵指数を得る。The dusting property was evaluated by the dusting index obtained by the following method. From the upper surface of the sample (heat-resistant structure) to the surface of the sample at a pressure of 3 × 10 4 N / m 2 , “Nichiban cellophane tape; C
T-24 width 24 mm "is attached. After standing for 5 seconds, the adhesive tape is peeled off from the sample. The peeled adhesive tape is attached on a black paper, and the brightness index is measured. The dust generation index is obtained by the following formula.
【００６７】発塵指数＝サンプルの明度指数−ブランク
の明度指数（ｎ＝５）
ここで、白色度とは、色彩色差計（形式「ＣＲ−３０
０」、測定ヘッド９１ｍｍ幅×２０１ｍｍ高さ×６０ｍ
ｍ奥行×６７０ｇ重量×測定径８ｍｍ、ミノルタ社製）
を用いて測定されれば良く、テープに付着する発塵の量
が多くなるにしたがって発塵指数は高い数値を示し、付
着する発塵の量が少ないほど低い数値を示す。また、ブ
ランクとは粘着テープに何も付着させない状態で黒色紙
上に貼り付けたときの明度指数を示す。Dust generation index = lightness index of sample-lightness index of blank (n = 5) Here, whiteness means a color difference meter (type "CR-30
0 ", measuring head 91mm width x 201mm height x 60m
m depth x 670 g weight x measurement diameter 8 mm, made by Minolta)
The dust generation index shows a higher numerical value as the amount of dust generated on the tape increases, and the lower the amount of dust generated, the lower the numerical value. The term "blank" refers to a lightness index when the adhesive tape is attached to black paper in a state where nothing is attached to the adhesive tape.
【００６８】また、平滑性の評価はＳＥＭによる観察で
行った。亀裂が発生せず、かつ表面形状が平坦になって
いるものを「◎」、亀裂は発生していないが表面形状が
やや劣っているものを「○」、亀裂が発生しているもの
や表面形状が著しく悪いものを「×」として評価した。The smoothness was evaluated by SEM observation. If there is no crack and the surface shape is flat, it is "◎"; if there is no crack, but the surface shape is a little inferior, it is "○". Those having a significantly bad shape were evaluated as “x”.
【００６９】[0069]
【表１】 [Table 1]
【００７０】表１に示すように、本発明による各実施例
の耐熱構造体はすべての評価ともに優れた結果が得られ
ている。しかし、比較例１の耐熱構造体では、使用に耐
えないレベルではないが亀裂が生じる。これは、１００
０℃を超えた温度条件で耐熱被覆層に含まれる有機バイ
ンダー由来の有機成分が揮発することに伴い、耐熱被覆
層に熱衝撃が加わり微細なクラックが生じてしまったと
考えられる。また、比較例２は、耐熱基材の熱膨張係数
に対して、耐熱被覆層の熱膨張係数が２５％を下回って
いるために、耐熱基材と耐熱被覆層との間で熱膨張差に
よる亀裂が発生し、全ての評価において不満足なものに
なっている。As shown in Table 1, the heat-resistant structures of the respective examples according to the present invention have excellent results in all evaluations. However, in the heat-resistant structure of Comparative Example 1, cracks are generated, although not at a level that can withstand use. This is 100
It is considered that as the organic components derived from the organic binder contained in the heat resistant coating layer volatilize under the temperature condition exceeding 0 ° C., thermal shock was applied to the heat resistant coating layer and fine cracks were generated. In Comparative Example 2, the coefficient of thermal expansion of the heat resistant coating layer is less than 25% with respect to the coefficient of thermal expansion of the heat resistant base material, so that the difference in thermal expansion between the heat resistant base material and the heat resistant coating layer results. Cracks occurred and were unsatisfactory in all evaluations.
【００７１】[0071]
【発明の効果】以上詳述したように、本発明によれば、
耐熱性に優れ、表面からの発塵がより抑制された耐熱構
造体を提供することができる。As described in detail above, according to the present invention,
It is possible to provide a heat resistant structure having excellent heat resistance and further suppressing dust generation from the surface.
フロントページの続き (72)発明者 吉本 俊裕 静岡県浜松市新都田１−８−１ Ｆターム(参考） 4K051 AA03 AB03 BD01 Continued front page (72) Inventor Toshihiro Yoshimoto 1-8-1 Shintoda, Hamamatsu City, Shizuoka Prefecture F-term (reference) 4K051 AA03 AB03 BD01
Claims (7)
熱構造体であって、前記耐熱被覆層は、粉末状耐熱材料
６０〜９０重量％と、無機バインダー５〜３０重量％
と、増粘材からなるコーティング剤とで形成されている
ことを特徴とする耐熱構造体。1. A heat resistant structure comprising a heat resistant base material and a heat resistant coating layer formed on the heat resistant base material, wherein the heat resistant coating layer comprises 60 to 90% by weight of a powdery heat resistant material and 5 to 30% by weight of an inorganic binder.
And a coating agent made of a thickening material, which is a heat-resistant structure.
％であることを特徴とする請求項１に記載の耐熱構造
体。2. The heat resistant structure according to claim 1, wherein the content of the thickener is 0.5 to 5% by weight.
のフュームドシリカであることを特徴とする請求項１ま
たは２に記載の耐熱構造体。3. The thickener has an average particle size of 5 to 40 nm.
3. The heat resistant structure according to claim 1, wherein the heat resistant structure is fumed silica.
の繊維状耐熱材料をさらに含むことを特徴とする請求項
１〜３のいずれかに記載の耐熱構造体。4. The coating agent is 1 to 20% by weight.
The heat resistant structure according to any one of claims 1 to 3, further comprising the fibrous heat resistant material.
シリカを主材とするコーティング層が形成されることを
特徴とする請求項１〜４のいずれかに記載の耐熱構造
体。5. The heat resistant structure according to claim 1, wherein a coating layer containing colloidal silica as a main material is formed on the surface of the heat resistant coating layer.
ティング層は、平均粒子径５０〜６００ｎｍのコロイダ
ルシリカ７０〜９５重量％と、無機バインダー５〜３０
重量％とからなるコーティング剤で形成されることを特
徴とする請求項５に記載の耐熱構造体。6. The coating layer containing colloidal silica as a main material comprises 70 to 95% by weight of colloidal silica having an average particle size of 50 to 600 nm and an inorganic binder of 5 to 30%.
The heat-resistant structure according to claim 5, wherein the heat-resistant structure is formed of a coating agent composed of 10% by weight.
れていることを特徴とする請求項１〜６のいずれかに記
載の耐熱構造体。7. The heat resistant structure according to claim 1, wherein the heat resistant substrate is formed of an inorganic molded body.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001393852A JP3992978B2 (en) | 2001-12-26 | 2001-12-26 | Heat-resistant structure |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001393852A JP3992978B2 (en) | 2001-12-26 | 2001-12-26 | Heat-resistant structure |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2003192472A true JP2003192472A (en) | 2003-07-09 |
| JP3992978B2 JP3992978B2 (en) | 2007-10-17 |
Family
ID=27600738
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2001393852A Expired - Fee Related JP3992978B2 (en) | 2001-12-26 | 2001-12-26 | Heat-resistant structure |
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| Country | Link |
|---|---|
| JP (1) | JP3992978B2 (en) |
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